Abstract: In this study the essential oils of Salvia officinalis growing in Sudan, were obtained by hydrodistillation and analyzed by Gas chromatography mass spectrometer, forty tow compounds were identified. The essential oil composition of S.officinalis found that it had many important compounds. The detected main compounds were oxygenated monoterpenes followed monohydrocarbone, squiterpenes and other compounds. The main essential oil constituents were α-terpineol (33.07%), camphor (11.57%), α-pinene (8.96%) camphene (5.09%) β-cymen (5.40 %) caryphyllene (3.76%) β-myrcene (3.65%) β-menth1-en-b-ol (3.45%) bomeol (3.38%) β-pinene (2.74%) Epiglobulol (2.59%) 1,8 Cineol (2.24%) and trans-β- terpinyl butanone(2.00% ).

Gas chromatography-coupled mass spectrometry (GC-MS) has been used in biomedical research to analyze volatile, non-polar, and polar metabolites in a wide array of sample types. Despite advances in technology, missing values are still common in metabolomics datasets and must be properly handled. We evaluated the performance of ten commonly used missing value imputation methods with metabolites analyzed on an HR GC-MS instrument. By introducing missing values into the complete (i.e., data without any missing values) NIST plasma dataset we demonstrate that Random Forest (RF), Glmnet Ridge Regression (GRR), and Bayesian Principal Component Analysis (BPCA) shared the lowest Root Mean Squared Error (RMSE) in technical replicate data. Further examination of these three methods in data from baboon plasma and liver samples demonstrated they all maintained high accuracy. Overall, our analysis suggests that any of the three imputation methods can be applied effectively to untargeted metabolomics datasets with high accuracy. However, it is important to note that imputation will alter the correlation structure of the dataset, and bias downstream regression coefficients and p-values.

The association between human and cat (F. catus) is well known. This domestic animal is also known for its malodorous urine and feces. The complexity of the odorous urine and feces impacts human life by triggering the human sensory organ in a negative way. The objective of this research was to identify the volatile organic chemicals (VOCs) and associated odors in cat urine and feces using gas chromatography-mass spectrometry and simultaneous sensory analysis of fresh and aged samples. The solid-phase microextraction (SPME) technique was used to pre-concentrate the VOCs emitted from urine or feces samples. Twenty-one compounds were identified as emitted from fresh urine, whereas 64 compounds were emitted from fresh feces. A contrasting temporal impact was observed on the emission of VOCs for urine and feces. On aging, the emission increased to 36 detected chemicals for stale urine, whereas only 17 chemicals were detected in stale feces. Not all compounds were malodorous; some compounds had a pleasant hedonic smell to the human nose. Although trimethylamine, low molecular weight organic acids, and ketones were contributors to the odor to some extent, phenolic compounds and aromatic heterocyclic organic N compounds generated the most intense odors and substantially contributed to the overall malodor, as observed by this study. This work might be useful to formulate cat urine and feces odor remediation approaches to reduce odor impacts.

In this study, GC–IMS was used to analyze the volatile component and flavor profiles of Crassostrea gigas individuals of different ploidy and gender. Principal component analysis was used to explore overall differences in flavor profiles and a total of 54 volatile compounds were identified. The total volatile flavor contents in edible parts of tetraploid oysters were significantly higher than in diploid and triploid oysters. The concentrations of ethyl (E)-2-butenoate and 1-penten-3-ol were significantly higher of triploid oysters than in diploid and tetraploid oysters. In addition, the volatile compounds propanoic acid, ethyl propanoate, 1-butanol, butanal, and 2-ethyl furan were significantly higher in females than in males. The volatile compounds p-methyl anisole, 3-octanone, 3-octanone, and (E)-2-heptenal were present in higher levels in male than in female oysters. Overall, different ploidy and gender of oysters were being presented with different sensory characteristics, providing new insights for understanding the flavor characteristics of oysters.

Glycosidic linkage analysis was conducted on the unfractionated polysaccharides in the alcohol-insoluble residues (AIRs) prepared from six red seaweeds (Gracilariopsis sp., Prionitis sp., Mastocarpus papillatus, Callophyllis sp., Mazzaella splendens, and Palmaria palmata) using GC-MS/FID analysis of partially methylated alditol acetates (PMAAs). The cell walls of P. palmata primarily contained mixed-linkage xylans and small amounts of sulfated galactans and cellulose. In contrast, the unfractionated polysaccharides of the other five species were rich in galactans displaying diverse 3,6-anhydro-galactose and galactose linkages with varied sulfation patterns. Different levels of cellulose were also observed. This glycosidic linkage method offers advantages for cellulose analysis over traditional monosaccharide analysis that is known for underrepresenting glucose in crystalline cellulose. Relative linkage compositions calculated from GC-MS and GC-FID measurements showed that anhydro sugar linkages generated more response in the latter detection method. This improved linkage workflow presents a useful tool for studying polysaccharide structural variations across red seaweed species. Furthermore, for the first time, relative linkage compositions from GC-MS and GC-FID measurements, along with normalized FID and total ion current (TIC) chromatograms without peak assignments, were analyzed using principal component analysis (PCA) as a proof-of-concept demonstration of the technique's potential to differentiate various red seaweed species.

Gasca D herbal formulation is an antidiabetic medicine for the management of diabetes mellitus produced exclusively from natural ingredients. The level of some essential elements (Copper, chromium, Cobalt, Iron, Manganese, Nickel and zinc) and toxic (Cadmium, Arsenic, Mercury, and Lead) heavy metals were determined using microwave plasma-atomic emission spectrometry (MP-AES). The aim of this study is to evaluate the levels of essential and toxic heavy metals and also identify bioactive compounds present in Gasca D herbal formulation. The result shows no traces of Lead, Mercury, Zinc, Arsenic and Zinc, Iron was found to have highest concentration 67.16 + 7.5 µg/g and Cadmium lowest concentration 0.4 + 0.03µg/g. GC-MS analysis of Gasca D herbal formulation revealed the presence of 14 biologically active compounds which include N-Formyl-beta-alanine, Paromomycin, 3,4-Altrosan, Benzamide, 1,3,4-Thiadiazol-2-amine, Carbamodithioic acid, Carbonic acid, alpha-D-Glucopyranoside, Ethyl isocyanide, 2-Propanesulfinic acid, Propanamide, 2-Butenenitrile, Dicyclopropyl carbinol, Isoxazolidine, 1,5-Hexadiene 10-Azido-1-decanethiol. Conclusion: The result indicates that the mean levels of toxic metals in Gasca D herbal formulation were below WHO permissible levels. Gasca D herbal formulation also contains various bioactive compounds that can have various medicinal application which can be used for the treatment of various diseases.

Exposure to malachite green (MG) may pose great health risks to humans, thus it is of prime importance to develop fast and robust methods to quantitatively screen the presence malachite green in environment. Herein application of extractive electrospray ionization mass spectrometry (EESI-MS) has been extended to the trace detection of MG within lake water and aquiculture water, due to the intensive use of MG as biocide in fisheries. This method has the advantage of obviating offline liquid-liquid extraction or tedious matrix separation prior to the measurement of malachite green in native aqueous medium. The experimental results indicate that the extrapolated detection limit for MG was ~3.8 ug L-1 (S/N=3) in lake water samples and ~ 0.5 ug L-1 in ultrapure water under optimized experimental conditions. The signal intensity of MG showed good linearity over the concentration range of 10–5000 ug L-1. Measurement of practical water samples fortified with MG at 0.01 and 0.1 mg L-1 gave a good validation of the established calibration curve. The average recoveries of malachite green in lake water and Carassius carassius fish farm effluent water were 114.9% (6.6% RSD) and 85.4% (9.2% RSD), respectively. Overall, the established EESI-MS/MS method has been demonstrated suitable for sensitive and rapid (<2 min per sample) quantitative detection of malachite green in various aqueous media, indicating its potential for online real-time monitoring of real life samples.

Essential oils are mixtures of compounds obtained from plants, including flowers, roots, bark, leaves, seeds,peel, fruits, wood, that have risen up in the last decades thanks to their beneficial properties as antibacterial, antifungal and anti-inflammatory agents. The aim of this study was to characterize and analyze 13 different commercial essential oils with two different techniques. The first is GC-MS, coupled with SPME, thanks to which 204 different VOCs have been identified. The results show that a total of 95 compounds was found only in one oil, while the others were found with different frequencies in many of them. The most represented class is that of terpenes, as widely reported in literature. The second technique is based on an array of chemical gas sensors. This system was used to investigate whether sensors are able to identify these products. It turned out that basil, cinnamon and carnation are the most identifiable oils with different number and typology of sensors, especially tin oxide and copper oxide nanowires, while cayeput and thyme are more mistakable samples. Thanks to this detailed study, it has been possible to reach and obtain novel insights for the future development of this type of research.

Tea (Camellia sinensis) is one of the most popular beverages worldwide. Many types of tea prod-ucts continuously emerge in an endless stream; so, the classification or verification of tea be-comes more difficult. Aroma is a vital indicator of tea quality. The present study deals with the identification of aroma compounds in 18 different kinds of tea belonging to three typical tea va-rieties, including green tea, oolong tea, and black tea, using GC-IMS and GC×GC-O-MS. More-over, the clustering of all 18 tea samples and the in-depth correlation analysis between sensory evaluation and instrumental data were performed using the PCA and OPLS-DA. The results re-vealed that in all 18 kinds of tea, a total of 85 aroma compounds were detected by GC-IMS, whereas 318 were detected by GC×GC-O-MS. The PCA result revealed that green tea, oolong tea, and black tea could be clearly separated based on their peak areas. The OPLS-DA result showed that a total of 49 aroma compounds with VIP value > 1.0 could be considered as the potential in-dicators to quickly classify or verify tea types. This study not only compared the aroma differ-ences across different types of teas, but also provided ideas for the rapid monitoring of tea qual-ity and variety.

The cooking method is extremely important for the production of low-salt, wet-marinated, fermented golden pomfret because it strongly influences its flavor components and organoleptic quality. There are also significant differences in flavor preferences in different populations. The present study analyzed differences in the aroma characteristics of wet-marinated fermented golden pomfret after boiling, steaming, microwaving, air frying and baking using a combination of an electronic nose, GC-IMS and SPME-GC-MS. Electronic nose PCA showed that the flavors of the boiled (A), steam (B) and microwave (C) treatment groups were similar, and the flavors of baking (D) and air frying (E) were similar. A total of 72 flavor compounds were detected in the GC-IMS analysis, and comparative analysis of the cooked wet-marinated and fermented golden pomfret yielded a greater abundance of flavor compounds. SPME-GC-MS analysis detected 108 flavor compounds, and the results were similar to the baking and air frying. Twelve key flavor substances, including hexanal, isovaleraldehyde, and (E)-2-dodecenal, were identified by orthogonal partial least squares discriminant analysis (OPLS-DA) and VIP analysis. These results show that cooking method is a key factor in the flavor distribution of wet-marinated fermented golden pomfret, and consumers can choose the appropriate cooking method accordingly.

Two-dimensional mass spectrometry (2D MS) is a method for tandem mass spectrometry that relies on manipulating ion motions to correlate precursor and fragment ion signals. 2D mass spectra are obtained by performing a Fourier transform in both the precursor ion mass-to-charge ratio (m/z) dimension and the fragment ion m/z dimension. The phase of the ion signals evolves linearly in the precursor m/z dimension and quadratically in the fragment m/z dimension. This study demonstrates that phase-corrected absorption mode 2D mass spectrometry improves signal-to-noise ratios by a factor of 2 and resolving power by a factor of 2 in each dimension compared to magnitude mode. Furthermore, phase correction leads to an easier differentiation between ion signals and artefacts, and therefore easier data interpretation.

Aim: Nepal’s medicinal plants are culturally important and have diverse benefits. Senna alata belongs to the family Leguminosae and is a valuable plant utilized for medicinal and ornamental purposes. The aim of the research was to extract Senna alata leaves by successive maceration with various solvents. Methods: In this study, various methods were utilized to evaluate phytochemistry, overall phenolic and flavonoid content, in-vitro antioxidant, anti-inflammatory, cytotoxicity assay, anti-thrombolytic activity, and antibacterial activities. Results: The extractive values of Senna alata were determined as 1.58%, 0.78%, and 5.92% in hexane, ethyl acetate, and methanol, respectively. GC-MS analysis revealed major compounds such as 3-Methylmannoside, Neophytadiene, Campesterol, and Vitamin E in the leaf extract. Qualitative phytochemical screening verified the tannin content, carbohydrates, flavonoids, cardiac glycosides, glycosides, and saponins in the methanol extract. The total phenolic and flavonoid values were 46.36±4.5 mg GAE/gm and 480.4±3.055 QE/gm of dried extract, respectively. The extract exhibited significant antioxidant and anti-inflammatory activities, with IC50 values of 29.81 and 9.93, respectively. Furthermore, it demonstrated cytotoxic activity with an LC50 value of 767.85 in the brine shrimp bioassay. In terms of thrombolytic activity, the extract showed clot lysis percentages of 7.89% and 10.13% at concentrations of 10 mg/ml and 25 mg/ml, respectively. Conclusion: In conclusion, the methanolic extract of Senna alata leaves displayed therapeutic potential, including antioxidant, anti-inflammatory, cytotoxic, thrombolytic, and antibacterial effects. The existence of several chemicals via GC-MS analysis also verified plant's potential for therapeutic use.

Currently, the pesticides are the global core concern because it is a boon to farmers against increasing disease-pest and simultaneously, pesticide residue is the major anxiety regarding human health. For that reason, identification and determination of factors affecting the application of pesticides are essential. To identify and evaluate determinants of pesticides application in Nepal, a household survey of 300 households was carried-out and an empirical analysis was done using multivariate probit model. Moreover, powder and liquid forms of pesticides were considered for summer and winter season in vegetable farming, which was assigned as outcome variables. Likewise, socio-economic, demographic, farm-level and perception data were considered as explanatory variables. Use of chemical fertilizers, age and gender of head of household, household size and access to weather information were found the most influencing factors. Moreover, forms of pesticides and growing seasons were found complementary to each other. Therefore, devising the policy options accordingly should balance needs of farmers and health of consumers.

Metabolomic analysis of biological fluids and tissues has become an increasingly routine tool in the biological toolbox. However, challenges remain to be overcome, including developing strategies to maximise coverage of the metabolome without requiring large sample volumes. Here we describe a multimodal strategy that combines data using both LC-MS and GC-MS from a unique vial with a sample of plasma (20µl) or a sample of brain tissue (3mg). Using a split phase extraction the non-aqueous phase was analyzed by reversed phase (RP) LC-MS, whilst the aqueous phase was analyzed using hydrophilic liquid interaction chromatography (HILIC)LC-MS, with both phases also analysed using GC-MS after derivatization of the extract. Analytical performance was assessed in 7 rat cerebellum samples and a pilot study of 40 plasma samples (20 vs. 20: AD vs. healthy controls). The method, which uses four hours of instrument time, measured 20,707 metabolite features in brain samples and 17,266 in plasma samples, from those 44.1% features displayed CV’s below 15% and 75.2% below 30%. The method has potential to resolve subtle biological differences and to correlate metabolite composition directly to clinical outcomes including MMSE, age and ADCS-ADL. This method can acquire in the order of 20K metabolic features when low volumes are available.

This study assessed farmers’ perception of climate change, estimated the determinants of, and evaluated the relationship among adaptation practices using the multivariate probit model. A survey in 300 agricultural households was carried out covering 10 sample districts considering five agro-ecological zones and a vulnerability index. Four adaptation choices (change in planting date, crop variety, crop type and investment in irrigation) were deemed as outcome variables and socioeconomic, demographic, institutional, farm-level and perceptions variables were deployed as explanatory variables. Their marginal effects were determined for three climatic variables—temperature, precipitation and drought. Age, gender and education of head of household, credit access, farm area, rain-fed farming and tenure, are found to be more influential compared to other factors. All four adaptation-options are found to be complimentary to each other. Importantly, the intensity of impact of dependent variables in different models, and for available adaptation-options, are found to be unequal. Therefore, policy options and support facilities should be devised according to climatic variables and adaptation options to achieve superior results.

Bioprospecting native Australian plants offers potential discovery of latent and novel bioactive compounds. Promising cytotoxic and antibacterial activity of methanolic extracts of Pittosporum angustifolium and Terminalia ferdinandiana led to further fractionation and isolation using our laboratory’s bioassay guided fractionation protocol. Hence, the aim of this study was to further evaluate the bioactivity of the fractions and subfractions and characterize bioactive compounds using liquid chromatography mass spectroscopy (LC-MS/MS) and gas chromatography MS (GC-MS). Compounds tentatively identified in P. angustifolium Fraction 1 using LC-ESI-QTOF-MS/MS were chlorogenic acid and/or neochlorogenic acid, bergapten, berberine, 8’-epitanegool and rosmarinic acid. GC-MS analysis data showed the presence of around 100 compounds, mainly comprising of carboxylic acids, sugars, sugar alcohols, amino acids, and monoalkylglycerols. Furthermore, the fractions obtained from T. ferdinandiana flesh extracts showed no cytotoxicity, except against HT29 cell lines, and only Fraction 2 exhibited some antibacterial activity. The reduced bioactivity observed in the T. ferdinandiana fractions could be attributed to the potential loss of synergy as compounds become separated within the fractions. As a result, further fractionation, and separation of compounds in these samples were not pursued. However, additional dose-dependent studies are warranted to validate the bioactivity of T. ferdinandiana flesh fractions, particularly since this is an understudied species. Moreover, LC-MS/GC-MS studies confirm the presence of bioactive compounds in P. angustifolium Fraction 1/subfractions which helps to explain the significant acute anti-cancer activity of this plant. The screening process designed in this study has the potential to pave the way for developing scientifically validated phytochemical/bioactivity information on ethnomedicinal plants, thereby facilitating further bioprospecting efforts, and supporting the discovery of novel drugs in modern medicine.

Fingerhuthia africana Lehm belongs to family Poaceae, is an erect perennial grass used traditionally to cure different diseases. The current study was carried out to find the bioactive compounds by GC-MS, elemental analysis through atomic absorption spectrophotometry, proximate analysis by AOAC, genotoxic activity through comet assay, antioxidant activity through DPPH and antidiarrheal activity through castor oil induce diarrhea followed by charcoal meal on mice model. GC-MS chromatogram represents different compounds detected in the crude extract. Major pharmacological bioactive compounds are 4H-Pyran-4-one, 2,3-dihydro-3,5-dihydroxy-6-methyl-; 4-Methyl itaconate; .alpha.-Terpineol; 1,2,3-Propanetriol, 1-acetate; Benzofuran, 2,3-dihydro-; Caryophyllene oxide; Hinesol; n-Hexadecanoic acid; 9,12-Octadecadienoic acid (Z,Z)-, methyl ester; Hexadecanoic acid and methyl ester. Elemental analysis of stem, leaves and roots of the plant show the presence of (macro and micro) nutrients such as Ca, Mg, K, Na, Cu, Pb, Zn, Mn, Fe, Cd and Co were absent in all parts. Proximate analysis of different parts revealed the presence of moisture contents (8.57%), ash (9.77%), fats contents (5.96%), fibers contents (45.03%), protein (3.62%), carbohydrates (39.71%) and Gross energy (Kcal/100g) (220.10). The ethanolic extract show dose-dependent genoprotective potential (127.38 ± 1.16), (83.28 ± 0.65), and (44.08 ± 1.40) at 50, 75, and 100 mg/100 ml, respectively, as compared to the methanolic extract which show genotoxic activity (85.13 ± 1.23) at high dose. After 90 minutes at a concentration of 300 (g/ml), methanolic extract demonstrated the greatest antioxidant potential (79.5%), followed by aqueous extract (76.5%). The methanolic extract of F. africana demonstrated antidiarrheal efficacy, with the maximum inhibition of charcoal movement (83.78%) occurring at a dosage of 300 mg/kg, followed by doses of 200 and 100 mg/kg, 73.26% and 59.56%, respectively. The current research highlights that the plant contains a substantial quantity of micro and macro nutrients, possesses high nutritional value, and exhibits pharmacological activities. These properties render the plant suitable for developing remedies to treat various therapeutic diseases.

Volatile organic compounds (VOCs) released from plants have been correlated with disease-status. Analysis of VOCs using GC-MS is time-consuming, laboratory-based, and requires specialist training. Electronic nose devices (E-nose) provide a portable alternative. Three different E-nose devices were compared to assess how accurately they could detect Mango Twig Tip Dieback and Panama disease in banana. The devices were initially trained on known volatiles, then pure cultures of Pantoea sp., Staphylococcus sp., and Fusarium odoratissimum, and finally, on infected and healthy mango leaves and field-collected, infected banana pseudo-stems. The experiments were repeated three times with six replicates for each host-pathogen pair. The variation between healthy and infected host materials was evaluated by principal component and linear discriminant analysis, cross-validation and chemometric data analysis. GC-MS analysis was conducted contemporaneously and identified an 80% similarity between healthy and infected plant material. The portable C 320 was 100% successful in discriminating known volatiles but had a low capability in differentiating healthy and infected plant substrates. The advanced devices (PEN 3 / MSEM 160) successfully detected healthy and diseased samples with a high variance. The results suggest that E-nose devices are more sensitive and accurate in detecting changes of VOCs between healthy and infected plants compared to headspace GC-MS.

Waterford Blaa is one of only seven Irish Protected Geographical Indication (PGI) products and the only Irish PGI bread. Currently, there are few published data characterising these products. This study aimed to determine whether any compositional or sensory markers could be used to differentiate between the three authorised producers of Waterford Blaa. Compositional testing was completed using AOAC standard methods; colour of top crust, bottom crust and crumb were identified with the Minolta Hunter lab colorimeter and texture profile analysis (TPA) was completed with an 80% compression test using the Instron 5544 to establish hardness, gumminess, and springiness. The fatty acid and aroma profiles were established in triplicate testing for the three authorised Blaa products using gas chromatography-flame ionisation detection and headspace-solid phase micro extraction-gas chromatography-mass spectrometry, respectively. As expected, results showed little variation in the overall composition of Waterford Blaa products. However, this study identified a unique fatty acid profile/volatile aroma profile for each Blaa. Specifically, the volatile profile showed potential differentiation between Blaa’s in terms of pentanal, furfural, 2-furanmethanol, 2-ethyl-1-hexanol and 2-pentyl furan. In addition, levels of hexanal and ethyl acetate were significantly different (p&lt;0.05) in the crumb section of all three Blaa’s. This unique fingerprint has the potential to be used to identify fraudulent products claiming to be Waterford Blaa.

The paper attempts to explore the relationship between federalism and rural development. Federalism is a division of power, responsibility and accountability to bring the administrative and political power closer to the ground and essentially to increase the good governance. On the other hand, rural development is a complex and multidimensional issue- especially much demanding for least developed and developing countries. A descriptive and qualitative approach was carried out to study the complex relationship between rural development and federalism. Similarly, a SWOT analysis was carried out to have a better understanding of the relationship. The study found that there is significant potentiality for accelerated development of rural landscape in federalism if carefully executed. However, on the other hand, federalism may pose several risks on rural development and may restrict the development pace if not executed with appropriate care and understanding. Therefore, the study concludes that cooperation and coordination among the federal structures are crucial for better development of the rural economy.

Citrus species essential oils (EOs) are significant sources of bioactive compounds and demonstrate diverse therapeutic effects. However, limited documentation exists regarding the phytochemicals associated with their biological activities. This study aims to assess the antioxidant activity, plant inhibitory properties, and brine shrimp cytotoxic effects of EOs derived from three Citrus species: C. sinensis, C. limon, and C. hystrix. Utilizing chemometric analysis and gas chromatography-mass spectrometry (GC-MS) fingerprints, the volatile components contributing to antioxidant activity were elucidated. The peels of the Citrus samples were hydro-distillated to obtain EOs, and subsequently subjected to antioxidant, plant inhibitory, and brine shrimp cytotoxic assays. The results indicated that C. limon EO exhibited the highest antioxidant activity, while C. hystrix and C. sinensis EOs demonstrated pronounced inhibitory effects against Aetrmia salina and Lactuca sativa, respectively. GC-MS analysis facilitated the identification of key compounds in each EO. Principal component analysis (PCA) and hierarchy cluster analysis (HCA) effectively categorized Citrus EOs based on their antioxidant properties, highlighting the proximity of C. limon and C. sinensis. Among the identified compounds, D-limonene, α-Terpineol, Caryophyllene, (+)-3-Carene, β-Pinene, (-)-Spathulenol, trans-p-Mentha-1(7),8-dien-2-ol, and trans-Verbenol were the most discriminating compounds affected the antioxidant activity of C.limon and C. sinensis EOs.

Dibutyl phthalate (DBP) is widely used as a plasticizer in the production of polymeric materials to give them flexibility, strength and extensibility. However, due to its negative impact on human health, in particular, reproductive function and fetal development, the content of DBP must be controlled in food and environmental objects. The present study aims to develop a sensitive, fast and simple polarization fluorescent immunoassay (FPIA) using monoclonal antibodies derived against DBP (MAb-DBP) for its detection in open waters. New conjugates of DBP with various fluorescein derivatives were obtained and characterized: 5-aminomethylfluorescein (AMF) and dichlorotriazinylaminofluorescein (DTAF). The advantages of using the DBP-AMF conjugate in the FPIA method are shown, the kinetics of binding of this drug with antibodies is studied, the analysis is optimized, and the concentration of monoclonal antibodies is selected for sensitive analysis - 16 nM. The calibration dependence of the fluorescence polarization signal for the detection of DBP was obtained. The observed IC50 (40 ng/mL) and LOD (10 ng/mL) values were improved by a factor of 35 for the previously described FPIA using polyclonal antibodies. This technique was tested by the added/found method, the percentage of DBP discovery in water ranged from 85 to 110%. Using the developed method, real water samples from Lake Onega were tested, and a good correlation was shown between the results of the determination of DBP by the FPIA method and GC-MS/MS. Thus, the FPIA method developed in this work can be used to determine DBP in open water reservoirs.

Breath volatile organic compound analysis is a non-invasive tool for assessing health status; the compositional profile of these compounds in the breath of patients with chronic kidney disease is believed to change with decreasing renal function. We aimed to identify breath volatile organic compounds for recognizing patients with chronic kidney disease. Using thermal desorption-gas chromatography-mass spectrometry, untargeted analysis of breath markers was performed using breath samples of healthy controls (n=18) versus non-dialysis (n=21) and hemodialysis (n=12) patients with chronic kidney disease in this cross-sectional study. A total of 303 volatile organic compounds alongside 12 clinical variables were used to determine the breath volatile organic compound profile. Metabolomic analysis revealed that age, systolic blood pressure, and fifty-eight breath volatile organic compounds differed significantly between the chronic kidney disease group (non-dialysis + hemodialysis) and healthy controls. Thirty-six volatile organic compounds and two clinical variables that showed significant associations with chronic kidney disease in the univariate analysis were further analyzed. Different spectras of breath volatile organic compounds between the control and chronic kidney disease groups were obtained. Multivariate model incorporating age, 2-methyl-pentane, and cyclohexanone showed high performance (accuracy, 86%) in identifying patients with chronic kidney disease, with odds ratios (95% confidence interval) P-values of 0.18 (0.07-2.49) 0.013; 2.10 (0.94-2.24) 0.025; and 2.31 (0.88–2.64) 0.008, respectively. Hence, renal dysfunction-associated characteristic profiles of breath volatile organic substances can be used as non-invasive markers to screen for chronic kidney disease.

Glycosphingolipids (GSL) represent a highly heterogeneous class of lipids with many cellular functions, implicated in a wide spectrum of human diseases. Their isolation, detection, and comprehensive structural analysis is a challenging task due to the structural diversity of GSL molecules. In this work, GSL subclasses are isolated from human plasma using an optimized monophasic ethanol–water solvent system capable to recover a broad range of GSL species. Obtained deproteinized plasma is subsequently purified and concentrated by C18-based solid-phase extraction (SPE). The hydrophilic interaction liquid chromatography (HILIC) coupled to electrospray ionization linear ion trap tandem mass spectrometry (ESI-LIT-MS/MS) is used for GSL analysis in the human plasma extract. Our results provide an in-depth profiling and structural characterization of glycosphingolipid and some phospholipid subclasses identified in the human plasma based on their retention times and the interpretation of tandem mass spectra. The structural composition of particular lipid species is readily characterized based on the detailed interpretation of MS and MS/MS spectra and further confirmed by specific fragmentation behavior following predictable patterns, which yields to the unambiguous identification of 154 GSL species within 7 lipid subclasses and 77 phospholipids representing the highest number of GSL species ever reported in the human plasma. The developed HILIC-ESI-MS/MS method can be used for further clinical and biological research of GSL in the human blood or other biological samples.

The genus Beauveria include important entomopathogenic and endophytic fungi, among them, Beauveria bassiana is the most studied species. However, there are few knowledge regarding their antimicrobial activity. The current research has been conducted to evaluate in vitro antagonistic activity of B. bassiana and the antimicrobial efficacy of its Exo and Endo metabolites against Bacillus cereus, B. megaterium, Clavibacter michiganensis (gram positive bacteria, G+ve), Xanthomonas campestris, Pseudomonas aeruginosa and P. fluorescence (gram negative bacteria, G-ve). In addition, Solid-phase microextraction (SPME) was coupled to Gas Chromatography-Mass Spectrometry (GC/MS) to qualitatively measure the volatile organic compounds (VOCs) metabolic profile of the most efficient studied isolate of B. bassiana. The obtained results showed that, the isolate UniB2439-3 has promising antibacterial effect against most of studied target bacteria. SPME-GC/MS analysis of VOCs revealed the presence of ethanol; butanal,2-methyl; 2,4-dimethyl-1-heptene; octane, 4-methyl and β-elemene as the main dominant bioactive compounds. The outgoing results explicated that the efficient isolate of B. bassiana can be potentially used as a biocontrol agent against several bacteria especially G+ve ones.

Tandem mass spectrometry (MS/MS) for diagnosing inborn errors of metabolism (IEM) is recognized as an ethical, safe, simple, and reliable screening test. Presented bibliometric analysis aims to describe the network structure of the scientific community in the study area at the level of countries, institutions, authors, papers, keywords, and sources; scientific productivity, directions, and collaboration efforts in a considered period (1991–2023.) Using the PRISMA method, we conducted a systematic search for articles reporting using MS/MS to screen for inherited metabolic disorders and inborn errors of metabolism collected from the Web of Science Core Collection (WOSCC.) A total of 451 articles out of 546, by 2,682 authors, published in 190 journals, with 15,440 citations in 8,181 citing articles, with an average citation of 34.24 per article, and an H-index of 64 were retrieved from the WOSCC. The research status of MS/MS in IEM screening was identified. The most relevant current research directions and future areas of interest were revealed: "selective screening for IEM," "new treatments for IEM," "new disorders considered for MS/MS testing," "ethical issues associated with newborn screening," "new technologies that may be used for newborn screening," "use of a combination of MS/MS and gene sequencing," etc.

Tributyltin (TBT) is one of the most toxic anthropogenic compounds introduced into the marine environment. Despite its global ban in 2008, TBT is still a problem of great concern due to its high affinity for particulate matter, providing a direct and potentially persistent route of entry into benthic sediments. Bioremediation strategies may constitute an alternative approach to conventional physicochemical methods, benefiting from the microorganism’s potential to metabolize anthropogenic compounds. In this work, a simple, precise and accurate static headspace gas chromatography method was developed to investigate the ability of TBT degrading microbes in sedimentary microcosms over a period of 120 days. The proposed method was validated for linearity, repeatability, accuracy, specificity, limit of detection and limit of quantification. The method was subsequently successfully applied for the detection and quantification of TBT and degrading compounds in sediment samples on day 0, 30, 60, 90 and 120 of the experiment employing the principles of green chemistry. On day 120 the concentration of TBT remaining in the microcosms ranged between 91.91 ng/g wet wt for the least effective microbial inoculant to 52.73 ng/g wet wt for the most effective microbial inoculant from a stating concentration of 100 ng/g wet wt.

A thorough analysis and comparison of the fatty acid profiles of stipe and blade from Laminaria hyperborea, a kelp species found in the northern Atlantic, is presented. Lipids were extracted and fractionated into neutral lipids, free fatty acids and polar lipids, then derivatized to fatty acid methyl esters prior to GC-MS analysis. A total of 42 fatty acids were identified and quantified, including the n-3 fatty acids α-linolenic acid, stearidonic acid and eicosapentaenoic acid. An n-6/n-3 ratio of 0.8:1 was found in blade and 3.5:1 in stipe, respectively. The ratios vary between the lipid fractions within stipe and blade, with the lowest ratio in the polar lipid fraction of blade. The fatty acid amounts are higher in blade than in stipe, and the highest amounts of n-3 fatty acids are found within the neutral lipid fractions. The amounts of polyunsaturated fatty acids are 3.4 times higher in blade than stipe. This study highlights the compositional differences between the lipid fractions of stipe and blade from L. hyperborea. The amount of polyunsaturated fatty acids, compared to saturated- and monounsaturated fatty acids, as well as the n-6/n-3-ratio, is known to influence human health. In the pharmaceutical, food, and feed industries this can be of importance for production and sale of different health products. Additionally, lipids are today among the unused by products of alginate production, exploiting this material for commercial interest should give both economical and environmental benefits.

(E)-β-ocimene was the only found volatile chemical emitted by whole, live worker larvae of Apis mellifera L. by sampling in the vapor phase. While in addition to (E)-β-ocimene, there is evidence for the existence of other volatiles; but the changes of their composition and contents remain unknown during larval development, as are their differences from larvae to larval food. This is the main purpose of the study. We investigated volatile components of worker larvae and larval food using solid phase dynamic extraction (SPDE) coupled with gas chromatography-mass spectrometry (GC-MS). Nine compounds were identified with certainty and six tentatively, consisting of terpenoids, aldehydes, hydrocarbons, ester and ketone. The contents of volatiles of the second-instar worker larvae differ greatly from larvae of other stages mainly attributable to terpenoids, which made the second-instar worker larvae had significantly higher amounts of overall volatiles. Larval food contained significantly higher amounts of aldehydes and hydrocarbons than the corresponding larvae from the fourth to fifth-instar. We discovered volatiles in worker larvae and their food which were never reported before; we also mastered the change of these volatiles’ contents during larval development.

Sensory descriptive analysis was used to evaluate the aged Feng-flavored baijiu. The results indicated that there are notable differences in the samples of different ages. The samples with shorter storage times and fresh distilled Baijiu present bran flavor, and fresh green flavor. with the increase of storage time, the fragrance of honey, sweetness, flowers, and aging gradually increases. The samples of Feng-flavored baijiu were dected by Headspace solid-phase microextraction (HS-SPME) combined with comprehensive two-dimensional gas chromatography time-of-flight mass spectrometry (GC×GC–TOFMS) , in total, 496 sustances were identified in all samples, mainly containing 14 types of substances, such as esters, aldehydes etc., of which 42 substances were found in Feng-flavored baijiu for the first time. Chemometrics was used to analyze the key differential compounds. 143 differential compounds closely related to aging were preliminarily screened, and principal component analysis revealed that these samples were separated by year. 65 differential compounds were selected out by partial least squares discriminant analysis(PLS-DA). Furthermore, 43 key differential compounds were selected from the aged Feng-flavored baijiu combined with variable importance in projection and Pearson correlation coefficients. Partial least squares regression (PLSR) was used to research the correlation of sensory properties and key differential compounds, and the results indicated that most compounds were closely related to the aged Baijiu . This study afford theoretical basis and reference for flavor research of Feng-flavored baijiu.

Culinary herbs and spices are widely used in daily diets. Pakistan flora is enriched with phytochemicals due to a diverse range of land. Phytochemicals, including volatile and non-volatile compounds, have captured much interest due to their numerous health advantages and significance in daily diet. The present study aimed to conduct in-depth metabolomic profiling of Pakistani-grown fenugreek leaves (Trigonella foenum-graecum), fennel seeds (Foeniculum vulgare), mint leaves (Mentha royleana), coriander seeds (Coriandrum sativum) and basil leaves (Ocimum basilicum) by using liquid chromatography–mass spectrometry (LC-MS/MS) and gas chromatography–mass spectrometry (GC-MS). The first study was conducted to optimize extraction using different solvents (methanol, ethanol, chloroform, acetone, and water). Total phenolic content (TPC), total flavonoid content (TFC), and total condensed tannins (TCT) were quantified along with the antioxidant and anti-diabetic activities. The highest TPC (125.42 ± 10.89 mg GAE/g) and the highest antioxidant and anti-diabetic potential were quantified in mint. Seventy-one phytochemical metabolites were identified using LC-MS/MS, while forty-nine volatile constituents were identified using the GC-MS. A positive correlation was identified between phenolic contents and their biological activities. Furthermore, molecular docking helped to find drug molecules with more excellent anti-diabetic activity based on their binding affinities. This study suggests that selected medicinal herbs from Pakistan have significant nutraceutical and phytopharmaceutical potential. This study could further help in drug discovery.

Onions are known not only for their culinary importance but also for their nutritional and health-promoting properties. Both properties are closely linked to its content of organosulfur compounds, which account for up to 5% of the dry weight of an onion. Given the importance of these compounds, suitable analytical methods are required for their study. Two techniques should be highlighted in this context: gas chromatography coupled to mass spectrometry (GC-MS), and liquid chromatography coupled to mass spectrometry (LC-MS). In this study, eight different onion varieties were analyzed using two distinct analytical techniques: direct thermal desorption–gas chromatography-mass spectrometry (DTD-GC-MS) and high-resolution mass spectrometry (HRMS) on an LC-ESI-QqTOF instrument. Each method identified 18 different organosulfur compounds, with LC-HRMS targeting non-volatile compounds, such as cysteine sulfoxides, and GC-MS targeting volatiles, such as disulfides and trisulfides. The results obtained were studied using Pearson correlations and principal component analysis. No precise correlation was found between the initial organosulfur compounds in onions and their hydrolysates. Consequently, although GC is one of the most employed techniques in the scientific literature, the use of LC-HRMS or a combination of both techniques may offer a more comprehensive and accurate description of the metabolomic profile of onions.

A novel determination method using flow-through cartridge purification and ultra-high-performance liquid chromatography coupled to tandem mass spectrometry (UPLC-MS/MS) was developed for the identification and quantification of 30 mycotoxins (aflatoxin B1, B2, G1, G2, sterigmatocysin, T-2 toxin, diacetoxyscirpenol, roquefortine C, methylergonovine, ergocornine, lysergol, enniatin A, enniatin A1, enniatin B, enniatin B1, beauvericin, deoxynivalenol, 3-acetylDeoxynivalenol, 15-acetylDeoxynivalenol, patulin, verruculogen, neosolaniol, gliotoxin, HT-2 toxin, wortmannin, zearalenone, α-zearalenol, β-zearalenol, α-zearalanol, and β-zearalanol) in feedstuffs. Mycotoxins were extracted from sample by 0.1% formic acid aqueous solution/acetonitrile (16/84 v/v), then purified by a Cleanert® MC clean-up column. As a result, the pigments and other matrices were efficient removed from the sample extract solution. The purified eluate was collected, then evaporated and redissolved by 0.1% formic acid aqueous solution/acetonitrile (70:30 v/v) for UPLC-MS/MS detection. A BEH Shield RP18 chromatographic column was employed for separation of 30 mycotoxins in a total of 14 min. Multiple-reaction monitoring (MRM) mode was applied for qualitative and quantitative analysis, and matrix calibration curves obtained with the external-standard method was used for quantitation of target analytes. Under optimized conditions, the linearity range was from 2 to 1000 ng/g, and the limit of quantification of the developed method was from 2 to 50 ng/g. The recoveries of 30 mycotoxins spiked in urine samples were from 72.0% to 118.5%, and the relative standard deviation was below 20%. The method was also well approved by certified reference sample, and applied on the real feedstuff samples testing successfully.

In this study, a new approach to pesticide permeation through the apple peel into the pulp is discussed. The tested compounds can be classified, based on mode of action, as systemic (boscalid, cyprodinil, pirimicarb, propiconazole and tebuconazole) or contact (captan, cypermethrin and fludioxonil) pesticides. The barrier effect was assessed using a Franz flow-type vertical diffusion cell system. Residue analysis was performed using a modified quick, easy, cheap, efficient, rugged and safe (QuEChERS) extraction method coupled to gas chromatography with tandem mass spectrometry (GC-MS/MS). The limits of detection (LODs) ranged between 2.6 µg kg-1 (pirimicarb) and 17 µg kg-1 (captan), with the coefficient of variability (CV) lower than 6%, while recoveries ranged from 85% (boscalid) to 112% (captan) at 0.1 and 1 mg kg-1 spiked levels. The highest peel penetration was observed for pirimicarb, captan and cyprodinil, with cumulative permeation of 90, 19 and 17 µg cm-2, respectively. The total absorption was in the range from 0.32% (tebuconazole) to 32% (pirimicarb). Only cypermethrin was not quantitatively detected in the pulp and its use can be recommended in crop protection techniques. The obtained results indicate that molecular weight, octanol-water partition coefficient and water solubility are important parameters determining the process of pesticide absorption.

Headspace solid phase microextraction (HS-SPME) coupled to gas chromatography-mass spectrometry is widely employed for volatile analyses of plants, including mapping populations used in plant breeding research. Studies often employ a single internal surrogate standard, even when multiple analytes are measured, with the assumption that any relative changes in matrix effects among individuals would be similar for all compounds, i.e. matrix effects do not show Compound × Individual interactions. We tested this assumption using individuals from two plant populations, an interspecific grape (Vitis spp.) mapping population (n = 140) and a tomato (Solanum spp.) recombinant inbred line (RIL) population (n = 148). Individual plants from the two populations were spiked with a cocktail of internal standards (n = 6, 9, respectively) prior to HS-SPME-GC-MS. Variation in the relative responses of internal standards indicated that Compound × Individual interactions exist but were different between the two populations. For the grape population, relative responses among pairs of internal standards varied considerably among individuals, with a maximum of 249% relative standard deviation (RSD) for the pair of [U13C]hexanal and [U13C]hexanol. However, in the tomato population, relative responses of internal standard pairs varied much less, with pairwise RSDs ranged from 8% to 56%. The approach described in this paper could be used to evaluate the suitability of using surrogate standards for HS-SPME-GC-MS studies in other plant populations.

The genus Beauveria include important entomopathogenic and endophytic fungi, among them, B. bassiana is the most studied species. However, there are few knowledge regarding their antimicrobial activity. The current research has been conducted to evaluate in vitro antibacterial efficacy of five isolates of B. bassiana against Bacillus cereus, B. megaterium, B. mojavensis, Clavibacter michiganensis (gram positive bacteria, G+ve), Xanthomonas campestris, X. vesicatoria, Escherichia coli, Pseudomonas aeruginosa and P. fluorescence (gram negative bacteria, G-ve). In addition, chemical composition of the principal diffusible metabolites and volatile organic compounds (VOCs) of the most efficient studied isolate of B. bassiana has been carried out using GC-MS analysis. The obtained results showed that, the isolate UniB2439-3 has promising antibacterial effect against most of studied target bacteria. GC-MS analysis of diffusible metabolites detected the presence of hexanedioic acid, bis(2-ethylhexyl) ester as the main compound in the cell-free culture filtrate. Furthermore, GC-MS analysis of VOCs revealed the presence of ethanol; butanal,2-methyl; 2,4-dimethyl-1-heptene; octane, 4-methyl and β-elemene as the main dominant bioactive compounds. The outgoing results explicated that, the isolates of B. bassiana have promising antibacterial activity which could be correlated to their diffusible and VOCs metabolites. Therefore, the selected isolate can be potentially used as a biocontrol agent against several bacteria especially G+ve ones. Taking in consideration that the antibiotics are forbidden in agriculture in many countries worldwide, search for possible natural alternatives as efficient antimicrobial agents are highly interesting.

Decoctions, macerations and fumigations of the stem bark and wood of Terminalia brownii Fresen. are used in traditional medicine for fungal infections and as pesticides on field crops and in traditional granaries in Sudan. In addition, T. brownii is commonly used for protecting wooden houses and furniture. Therefore, using agar disc diffusion and macrodilution methods, eight extracts of various polarities from the stem wood and bark were screened for their growth inhibitory effects against filamentous fungi commonly causing fruit, vegetable and grain decay, as well as infections in the immunocompromised host. Ethyl acetate extracts of the stem wood and bark gave the best antifungal activities, with MIC values of 250 µg/ml against Nattrassia mangiferae and Fusarium verticillioides, and 500 µg/ml against Aspergillus niger and Aspergillus flavus. Aqueous extracts gave almost as potent effects as the ethyl acetate extracts against the Aspergillus and Fusarium strains, and were slightly more active than the ethyl acetate extracts against Nattrassia mangiferae. Thin layer chromatography, RP-HPLC-DAD and tandem mass spectrometry (LC-MS/MS), were employed to identify the chemical constituents in the ethyl acetate fractions of the stem bark and wood. The stem bark and wood were found to have a similar qualitative composition of polyphenols and triterpenoids, but differed quantitatively from each other. The stilbene derivatives, cis- (3) and trans- (4) resveratrol-3-O-β-galloylglucoside, were identified for the first time in T. brownii. Moreover, methyl-(S)-flavogallonate (5), quercetin-7-β-O-di-glucoside (8), quercetin-7-O-galloyl-glucoside (10), naringenin-4`-methoxy-7-pyranoside (7), 5,6-dihydroxy-3`,4`,7-tri-methoxy flavone (12), gallagic acid dilactone (terminalin) (6), a corilagin derivative (9) and two oleanane type triterpenoids (1) and (2) were characterized. Our results justify the traditional uses of macerations and decoctions of T. brownii stem wood and bark for crop and wood protection and demonstrate that standardized extracts could have uses for the eco-friendly control of plant pathogenic fungi in African agroforestry systems. Likewise, our results justify the traditional uses of these preparations for the treatment of skin infections caused by filamentous fungi.

Parmigiano Reggiano cheese is one of the most appreciated and consumed food worldwide, especially in Italy, for its high content of nutrients and for its taste. However, these characteristics make this product subject to counterfeiting in different forms. In this study, a novel method based on an electronic nose has been developed in order to investigate the potentiality of this tool to distinguish rind percentage in grated Parmigiano Reggiano packages that should be lower than 18%. Different samples in terms of percentage, seasoning and rind working process were considered to tackle the problem at 360°. In parallel, GC-MS technique was used to give a name to the compounds that characterize Parmigiano and to relate them with sensors responses. Data analysis consisted of two stages: multivariate analysis (PLS) and classification made in a hierarchical way with PLS-DA ad ANNs. Results are promising in terms of correct classification of the samples. The classification rate is higher for ANNs than PLS-DA, reaching also 100% values.

Elephant dung coffee (Black Ivory Coffee) is a special Thai coffee produced from Arabica coffee cherries consumed by Asian elephants and collected from their feces. In this work, elephant dung coffee and controls were analyzed using static headspace gas chromatography hyphenated with mass spectrometry (SHS GC–MS), and chemometric approaches were applied for multivariate analysis and the selection of marker compounds that are characteristic of the coffee. Seventy-eight volatile compounds belonging to 13 chemical classes were tentatively identified, including 6 alcohols, 5 aldehydes, one carboxylic acid, 3 esters, 17 furans, one furanone, 13 ketones, 2 oxazoles, 4 phenolic compounds, 14 pyrazines, one pyridine, 8 pyrroles and 3 sulfur-containing compounds. Moreover, four potential discriminant markers of elephant dung coffee, including 3-methyl-1-butanol, 2-methyl-1-butanol, 2-furfurylfuran and 3-penten-2-one were established. The proposed method may be useful for elephant dung coffee authentication and quality control.

The majority of the population in developing countries resides in the rural area. Development itself cannot address the challenges of the rural area since its economic, political and environmental landscape is different from an urban area. The paper attempts to assess the rural dimension aspect of Nepali Agriculture Policy since rural development and agricultural development is closely resembled due to an agrarian-based economy of the country and a large rural population. Therefore, a critical review of National Agriculture Policy, 2004 (NAP-2004) was carried out under “Commercialization of Agriculture”, “Food Security”, “Rural Infrastructure”, “Gender”, “Climate Change” and “Social Inclusion” thematic area. The results showed that NAP-2004 satisfactorily address rural development albeit ample space for improvement. The findings of the paper could be beneficial to policymakers and development workers in the field of rural development and agriculture along with academicians having interest in it.

A convenient and fast multiresidue method for the efficient identification and quantification of 72 pesticides belonging to different chemical classes in red and white grape wines have been developed. The analysis was based on gas chromatography tandem quadrupole mass spectrometric determination (GC–MS/MS). An optimization strategy involved the selection of MWCNTs amount and cleanup procedure cycle times for m-PFC was performed to achieve ideal recoveries and reduce sample matrix compounds in the final extracts. The optimized procedure obtained consistent recoveries between 70.2 and 108.8% (70.2% and 108.8% for white wine, 72.3% and 106.0% for red wine) , with relative standard deviations (RSDs) generally lower than 8.3% at three spiking levels of 0.01, 0.05 and 0.2 mg/kg. Linearity was studied in the range between 0.005 and 0.2 mg/kg using pesticide standards prepared both in pure solvent and in the presence of matrix, showing coefficients of determination (R²) higher than 0.985 for all the pesticides. To improve accuracy, matrix matched calibration curves were used for calculating the quantification results. Finally, the method was used successfully in detecting pesticide residues in commercial gape wines.

Fabric phase sorptive extraction, an innovative integration of solid phase extraction and solid phase microextraction principles, has been combined with gas chromatography-mass spectrometry for the rapid extraction and determination of nineteen organochlorine pesticides in various fruit juices and water samples. FPSE consolidates the advanced features of sol-gel derived extraction sorbents with the rich surface chemistry of cellulose fabric substrate, which could directly extract target analytes from complex sample matrices and substantially simplifies the sample preparation operation. Important FPSE parameters including sorbent chemistry, extraction time, stirring speed, type and volume of back-extraction solvent and back-extraction time have been optimized. Calibration curves were obtained in the concentration range 0.1-500 ng/mL. Under the optimum conditions, the limits of detection were obtained in the range 0.007-0.032 ng/mL with satisfactory precision (RSD<6%). The relative recoveries obtained by spiking organochlorine pesticides in water and selected juice samples were in the range of 91.56–99.83%. The sorbent sol-gel poly(ethylene glycol)-poly(propylene glycol)-poly(ethylene glycol) was applied for the extraction and preconcentration of organochlorine pesticides in aqueous and fruit juice samples prior to analysis with gas chromatography-mass spectrometry. The results demonstrated that the present method is simple, rapid, and precise for the determination of organochlorine pesticides in aqueous samples.

Gas chromatography-olfactometry/mass spectrometry coupled with headspace-solid phase microextraction (HS-SPME/GC-O/MS) was applied for the characterization of volatile compounds in Tom Yum soup and its individual ingredients. Using HS-SPME with a 50/30 µm DVB/CAR/PDMS fiber and an extraction temperature of 40 °C for 50 min along with an HP-5MS capillary column, 101 peaks in the HS-SPME/GC-MS chromatogram of Tom Yum soup were detected, and 96 compounds were identified including alcohols, aldehydes, esters, ethers, and terpenes. These findings are based on the comparison of MS spectra with the NIST library as well as experimental and literature retention index data. In comparison with the compound profiles of each individual ingredient of Tom Yum soup (both before and after cooking), five extra volatile compounds in Tom Yum soup were found after the cooking process. Furthermore, odor descriptions of the eighteen aroma compounds in Tom Yum soup, along with the odor ingredient sources, were also obtained.

Bacillus species produce different classes of antimicrobial and antioxidant substances: peptides or proteins with different structural composition and molecular mass and a broad range of volatile organic compounds (VOCs), some of which may serve as biomarkers for microorganism identification. The aim of this study is the identification of biologically active compounds synthesized by five Bacillus species using gas chromatography coupled to mass spectrometry (GC–MS). The current study profoundly enhances the knowledge of antibacterial and antioxidant metabolites ensuring the unambiguous identification of VOCs produced by some Bacillus species, which were isolated from vegetable samples of potato, carrot, and tomato. Phylogenetic and biochemical studies were used to identify the bacterial isolates after culturing. Phylogenetic analysis proved that five bacterial isolates BSS12, BSS13, BSS16, BSS21, and BSS25 showed 99% nucleotide sequence similarities with Bacillus safensis AS-08, Bacillus cereus WAB2133, and Bacillus acidiproducens NiuFun, Bacillus toyonesis FORT 102 and Bacillus thuringiensis F3, respectively. The crude extract was prepared from bacterial isolates to assess the antibiotic resistance potency and the antimicrobial potential against various targeted multidrug-resistant strains, including Candida albicans, Candida krusei, Enterococcus hirae, Escherichia coli, Klebsiella aerogenes, Klebsiella pneumoniae, Staphylococcus aureus, Staphylococcus epidermidis, Streptococcus group B, Streptococcus mutans, Shigella sonnei, Salmonella enteritidis, Serratia marcescens, Pseudomonas aeruginosa, and Proteus vulgaris. GC–MS analysis of bacterial strains found that VOCs from Bacillus species come in a variety of chemical forms, such as ketones, alcohols, terpenoids, alkenes, etc. Overall, 69 volatile organic compounds were identified from five Bacillus species, and all five were found to share different chemical classes of volatile organic components, which have a variety of pharmacological applications. However, 8 antibacterial compounds with different concentrations were commonly found in all five species: acetoin, acetic acid, butanoic acid, 2-methyl-, oxime-, methoxy-phenyl, phenol, 1,2-benzenedicarboxylic acid, bis(2-methylpropyl) ester, nonanoic acid, and hexadecanoic acid, methyl. The biology and physiology of Bacillus can be better understood using these results, which can also be used to create novel biotechnological procedures and applications. Moreover, because of its exceptional ability to synthesize and produce a variety of different antibacterial compounds, Bacillus species can serve as natural and universal carriers for antibiotic compounds in the form of probiotic cultures and strains to fight different pathogens, including mycobacteria.

Secondary metabolites are bioactive compounds produced by living organisms that can reveal symbiotic relationships in nature. In the work described here, soil-born entomopathogenic-nematodes associated with symbiotic bacteria (Xenorhabdus stockiae and Photorhabdus luminescens) extracted from solvent supernatant containing secondary metabolites showed significant inhibitory action against Escherichia coli, Staphylococcus aureus, Enterococcus faceium, Proteus vulgaris, Bacillus cereus, Bacillus subtilis. These secondary metabolites, characterized by Fourier transform infrared spectroscopy were found to be amine groups of proteins; hydroxyl and carboxyl groups of polyphenols; hydroxyl groups of polysaccharides, and carboxyl groups of organic acids. The major compounds identified by Gas chromatography-mass spectrometry analysis of ethyl acetate extracts of Xenorhabdus stockiae revealed the existence of Nonanoic acid derivatives, Paromycin, Pyrrolidinone, Octodecanal derivatives, Trioxa-5-aza-1-silabicyclo, 4-Octadecenal, Methyl ester, Oleic Acid and 1,2-benzenedicarboxylicacid. Additional extraction from Photorhabdus luminescens was expressed functional compounds such as Indole-3-acetic acid, Piperidinol derivatives, Phthalic acid, 1-Tetradecanol, Nemorosonol, 1-eicosanol and unsaturated fatty acids. These outcomes support the development of new alternative natural antimicrobial agents for pathogen suppression in the future.

Plasma and serum are the most widely used blood-derived biofluids for metabolomics and lipidomics assays, but the isolation of these products from blood may introduce additional bias as indicated by the fact that many analytes that are present at high concentrations in blood cells cannot be measured and evaluated in those samples. Of particular concern, variable hemolysis during the pre-processing of blood products could compromise accurate and reproducible quantification. Compared with plasma or serum, whole blood may be a better alternative due to simplicity of processing. In this study, we provide a comprehensive method for quantification of the whole blood sphingolipidome and the concentrations were compared with those from plasma. Combining a single-phase extraction method with liquid-chromatography high resolution mass spectrometry (R=120, 000), assisted by alkaline hydrolysis, we were able to identify and simultaneously quantify more than 150 sphingolipids. Furthermore, most of sphingolipids remained stable after a freeze/thaw cycle. Whole blood contained a higher concentration of most sphingolipids than corresponding plasma. Moreover, individual variations in the levels of sphingolipids were lower for whole blood than plasma. These findings demonstrate that whole blood could be a better alternative to plasma, and potentially guide the evaluation of sphinglipidome for biomarker discovery.

In this study, a three-dimensional bioelectrochemical reactor system (3D-BERs) with granular activated carbon (GAC) epitomizes a novel treatment technology for treating nitrate-polluted water. The conventional denitrification process faces many challenges, including the huge demand for organic carbon, long-term accumulation of intermediate products, and the adaptation period. Results shown that under the optimal conditions of the COD/NO3--N ratio was 1.5, the denitrification efficiency reached 98.62%, when compared to 81.12% at COD/ NO3--N ratio of 3.5, and the initial pH of 7.5 ± 0.5, NO3--N was entirely removed at 2.2 h without accumulation of nitrite. The high initial ratio of NO2--N/NO3--N is mainly to accelerate the denitrification rate by accelerating the reduction of nitrite. Denitrification process followed by zero-order kinetics linear model for at different concentrations of inlet NO3--N, and achieved higher denitrification rate at greater inlet NO3--N concentration. High-throughput sequencing shows that the community structure and relative abundance of bacteria changed significantly, especially at the genes and the phyla level in immobilized GAC particles. Microbial composition enhanced the removal of nitrogen at the inner surface (IS) and bottom surface (BS) of immobilized GAC carriers. Therefore, this system is expected to be a more efficient and useful supplement or a cost-effective alternative compared to the traditional low carbon to nitrogen wastewater treatment system.

The presence of antibiotic residues in honey has recently become a growing public health concern due to the overuse of these products in beekeeping and their transfer to the food industry. The aim of this study was to develop and validate a simple, selective and sensitive method for the simultaneous identification and quantification of residues of twenty-two sulfonamides, trimethoprim and dapsone in honey using a rapid and reliable liquid chromatography–tandem mass spectrometry (LC–MS/MS) method. The developed method showed good linearity, specificity, precision (repeatability and intra-laboratory reproducibility) and recovery. The decision limit (CCalpha) ranged between 2.16-22.12 µg/kg for CCα, while the detection capability (CCbeta) was between 2.16- 2.67-27.36 µg/kg. The method proved to be rapid, reliable and effective for the determination of sulfonamides, trimethoprim and dapsone from honey samples. The average recoveries were estimated to be between 70 and 106%. The relative standard deviations (RSDs) were between 6-18%. In practice, the method is essential to check the honey sold on the market and ensure its safety before it reaches the consumer.

SPME analysis of the scent Ophrys orchids gave the following results: O. apifera: benzyl benzoate, -copaene, caryophyllene, and cyclosativene. O. crabronifera subsp. biscutella: pentadecene, pentadecane, heptadecane, nonadecane, and heinecosane. O. bertolonii subsp. bertolonii: pentadecane, heptadecane and nonadecane. O. passionis subsp. garganica: i-propyl palmitate, caryophyllene, pentadecane, and heptadecane. O. holosericea subsp. apulica: -copaene, pentadecane, caryophyllene, and heptadecane. O. lacaitae: -copaene, pentadecane, heptadecane, and caryophyllene. O. bombyliflora: cyclosativene, pentadecane, and ethyl dodecanoate. O. insectifera: 8-heptadecene, pentadecane, and heptadecane. O. lutea: heptadecane, 8-heptadecene, nonadecane, and docosane. O. tenthredinifera subsp. neglecta: -copaene, caryophyllene, and i-propyl palmitate.

Scientific advancements in the food industry have resulted in the discovery of natural substances that can serve various functions in food. Essential oils, in particular, can act as food preservatives or flavoring agents due to their abundance of natural antioxidants, which possess preservative properties. In this study, the composition of Thymus vulgaris essential oil was determined using GC-MS and HS-SPME. The essential oil obtained from Thymus vulgaris L. through hydro-distillation yielded approximately 4%. GC/MS analysis of the essential oil identified 11 components, with a predominant presence of oxygenated monoterpenes (56.97%). Notably, carvacrol (37.63%) and thymol (17.35%) were present in significant amounts, accounting for 54.98% of the overall composition. The in vitro antioxidant activity of the essential oil was evaluated using three methods. The DPPH free radical scavenging test yielded an IC50 of 0.51±0.11 mg mL-1. The β-carotene/linoleic acid bleaching test resulted in an IC50 of 2.58±0.10 mg mL-1. Finally, the ABTS assay indicated relatively lower antioxidant activity compared to ascorbic acid.

Hang-ju was one of five officinal varieties of Flos chrysanthemum for its edible and potable usage. Besides Flos Chrysanthemum (FL), there were also Bud Chrysanthemum (BC) and Fetal Chrysanthemum (FC) at the early and late stage of buds, respectively, in the consumption market of Hang-ju with higher prices. Whether the quality and efficiency of BC and FC was superior to FL or merely consumption misunderstandings? Three commercial products of Hongxinju, a representive cultivar of Hang-ju were studied with a GC-MS based metabolomics approach, complemented with morphology, contents of moisture and protein and the anti-oxidant activity, to reveal the metabolic alterations of violate components in Hongxinju in different flowering stage and at different processing periods. It revealed that most of the violate components were increased from fresh FC to FL, and the low-boiling fractions, inflammatory methyl arachidonate and air-polluting component of ethylbenzene were declined while the representative components with pungent flavor and cool nature of a-curcumene and (Z,Z,Z)-9,12,15-octadecatrienoic acid, vision improving carotenol of rhodopin and high-boiling fractions were elevated after processed in final FL compared with that in BC and/or FC. Though the content of protein and anti-oxidative capacity of final BC and FC were nearly equal to those of FL, in comprehensive consideration of the representative components related with the efficiency in heat cooling and vision improving, as well as the representative components related with inflammation and air-pollution, final FL was recommended other than BC and FC in the practice of medicine with the yield and quality integrated into account.

The blue sepal color of hydrangea is due to a metal complex anthocyanin composed of 3-O-glucosyldelphinidin (1) and an aluminum ion with the co-pigments 5-O-caffeoylquinic acid (2) and/or 5-O-p-coumaroylquinic acid (3). The three components, namely, anthocyanin, Al³⁺ and 5-O-acylquinic acids, are essential for blue color development, but the complex is unstable and only exists in aqueous solution. Furthermore, the complex did not give analyzable NMR spectra or crystals. Therefore, many trials to determine the detailed chemical structure of the hydrangea-blue complex have failed to date. Instead, via experiments mixing 1, Al³⁺ and 2 or 3 in a buffered solution at pH 4.0, we obtained the same blue solution derived from the sepals. However, the ratio was not stoichiometric but fluctuated. To determine the composition of the complex, we tried direct observation of the molecular ion of the complex using electrospray-ionization mass spectrometry. In a very low-concentration buffer solution (2.0 mM) at pH 4.0, we reproduced the hydrangea-blue color by mixing 1, 2 and Al³⁺ in ratios of 1:1:1, 1:2:1 and 1:3:1. All solution gave the same molecular ion peak at m/z = 843, indicating that the blue solution has a ratio of 1:1:1 for the complex. By using 3, the observed mass number was m/z = 827 and the ratio of 1, 3 and Al³⁺ was also 1:1:1. A mixture of 1, 3-O-caffeoylquinic acid (4) and Al³⁺ did not give any blue color but instead was purple, and the intensity of the molecular ion peak at m/z = 843 was very low. These results strongly indicate that the hydrangea blue-complex is composed of a ratio of 1:1:1 for 1, Al³⁺ and 2 or 3.

Accurate determination of the concentration of alcohols and their metabolites is important in forensics and in several life science areas. A new method has been developed to quantify alcohols and their oxidative products using a headspace gas chromatography- mass spectrometer and isotope-labelled internal standards. This work demonstrates the application of this method, specifically in quantifying the concentration of oxidative products of alcohol and other minor alcohols found in hand sanitizers, which have become an essential household item since the COVID-19 pandemic. Apart from the major component, the minor alcohols found in hand sanitizers include methanol, isopropanol, and n-propanol. In ethanol-based hand sanitizers, a significant amount of acetaldehyde was observed as an oxidation product, while in isopropanol-based hand sanitizers, acetone was observed. The concentration of acetaldehyde in ethanol-based hand sanitizers significantly increased with storage time and temperature, whereas no such increase of acetone concentration was observed in isopropanol-based hand sanitizers with storage time and temperature.

In the last decade, the tremendous improvement in the sensitivity and also affordability of Liquid Chromatography-tandem Mass Spectrometry (LC-MS/MS) have revolutionized its application in pharmaceutical analysis, resulting in wide-spread of employing LC-MS/MS for determining pharmaceutical compounds including anticancer drugs in pharmaceutical research and also industries. Currently, LC-MS/MS has been widely used to quantify small molecule oncology drugs in various biological matrices to support preclinical and clinical Pharmacokinetic studies in R & D of oncology drugs. This mini-review article will describe the state-of-the art LC-MS/MS and its application in rapid quantification of small molecule anticancer drugs. In addition, efforts have also been made in this review to address several key aspects in the development of rapid LC-MS/MS methods, including sample preparation, chromatographic separation and matrix effect evaluation.

This study aimed to determine the Gas Chrommatography (GC)-Mass Spectrometry (MS) profiles and insecticidal activity of essential oils (EOs) from Thymus vulgaris (Thyme) and Cymbopogon citratus (Lemongrass) against the invasive and devastating pest, Tuta absoluta (T. absoluta) through contact and fumigation routes. We found out that thyme oil was predominantly constituted of Thymol (22.16%), α-Pinene (15.35%) and p-Cymene (13.54%) whilst Neral (21.41%), Geranial (21.36%) and β-Myrcene (9.74%) were the major constituents of lemongrass oil. Lemongrass oil exhibited higher insecticidal efficiency irrespective of application mode with 50% lethal dose (LD50) values of 35.8 and 72.2 µL.L-1air on contact and fumigation routes, respectively. Lemongrass oil also lengthened pupal duration at all tested doses irrespective of application routes. The overall responses of Lemongrass oil surpassed that of the reference insecticide (Lynx®: Lambda-cyhalothrine; Acetamipride). Thus, the recorded data clearly showed the acute and long-term insecticidal effects of the studied EOs, though a greenhouse and open field trials are required prior to the validation of this approach as remediation measure for Integrated Pest Management (IPM) for tomato borer control in Cameroon and elsewhere.

The surge in popularity of Delta-8 Tetrahydrocannabinol (D8-THC) products, coupled with a lack of stringent regulation and oversight, has given rise to concerns regarding consumer safety and compliance with existing laws. This article delves into the challenges posed by the unregulated sale of D8-THC products, emphasizing the potential for contamination with prohibited constituents, including Delta-9 Tetrahydrocannabinol (D9-THC). The 2018 Farm Bill dictates that D9-THC concentrations must not exceed 0.3%, necessitating precise testing methods for accurate validation. Existing testing procedures, particularly involving High-Performance Liquid Chromatography (HPLC), face difficulties in distinguishing between D8 and D9 peaks, necessitating adjustments in parameters to enhance accuracy. The development of more refined testing methodologies is crucial for companies to ensure compliance, prevent adverse health effects, and provide consumers with accurately characterized cannabinoid profiles in the products they purchase.

Synthetic cannabinoids are a series of synthetic substances that mimic the effects of natural cannabinoids and produce a much stronger toxicity than natural cannabinoids, which have become the most abused family of new psychoactive substances. A solid-phase extractive-liquid chromatography-triple quadrupole/linear ion trap mass spectrometry method was developed to determine 11 synthetic cannabinoids in rat urine. The factors affecting recovery were optimized, and Oasis HLB was selected to extract synthetic cannabinoids simultaneously. The results showed that the linear correlation coefficients of the synthetic cannabinoids ranged from 0.993 to 0.999, and the limit of quantitation ranged from 0.01 to 0.1 ng/mL, and the spiked recoveries ranged from 69.90% to 118.39%. This method has the advantages of good purification ability, simple operation, and good reproducibility, and can be used for the high sensitivity analysis of various synthetic cannabinoids in urine.

Coptisine (Cop) exerts a neuroprotective effect in central nervous system disease, particularly ischemic stroke. However, its protective mechanism is still unclear. This study aimed to investigate the protective effect of Cop on cerebral ischemia-reperfusion (IR) rats with a middle cerebral artery occlusion model by integrating a gas chromatography-mass spectrometry (GC-MS) based metabolomics approach with biochemical assessment. Our results showed that Cop could improve neurobehavioral function and decrease the ischemia size in IR rats. In addition, Cop was found to decrease inflammatory mediators (e.g., prostaglandin D2 (PGD2) and tumor necrosis factor-α (TNF-α) and attenuate oxidative stress response (e.g., increase the superoxide dismutase (SOD) expression and decrease 8-iso-PGF2α level). Furthermore, GC-MS based cerebrospinal fluid (CSF) metabolomics analysis indicated that Cop influenced the level of glycine, 2,3,4-trihydroxybutyric acid, oleic acid, glycerol, and ribose during IR injury. Cop exhibited a good neuroprotective effect against cerebral IR injury and metabolic alterations which might be mediated through its antioxidant and anti-inflammatory property.

Diesel contamination of farming soils is of great concern because hydrocarbons are toxic to all forms of life and can potentially enter the food web through crops or plants used for remediation. Data on plant ability to uptake, translocate and accumulate diesel-derived compounds are controversial not only due to the probable diverse attitude of plant species but also because of the lack of a reliable method to distinguish petrogenic from biogenic compounds in plant tissues. The purpose of this study was to set up a GC-MS-based protocol enabling the determination of diesel-derived hydrocarbons in plants grown in contaminated soil for assessing human and ecological risks, predicting phytoremediation effectiveness and biomass disposal. To this aim two plant species Vicia sativa L. and Secale cereale L., belonging to two diverse vascular plant families, were used as plant models. They were grown in soil spiked with increasing concentrations of diesel fuel and the produced biomass was used to set up the hydrocarbon extraction and GC-MSD analysis. The developed protocol was also applied to the analysis of Typha latifolia L. plants, belonging to a different botanical family and grown in a long-time and highly contaminated natural soil. Results showed the possibility of distinguishing diesel-derived compounds from biogenic hydrocarbons in most terrestrial vascular plants, just considering the total diesel compounds in the n-alkanes carbon range C10-C26, where the interference of biogenic compounds is negligible. Diesel hydrocarbons quantification in plant tissues was strongly correlated (0.92<r2<0.99) to the concentration of diesel in spiked soils, suggesting a general ability of the considered plant species to adsorb and translocate relative low amounts of diesel hydrocarbons and the reliability of the developed protocol.

Matrix-assisted laser desorption/ionization time-of-flight mass spectrometry (MALDI–TOF MS) is a commonly used technique for analyzing large biomolecules. However, the utilization of organic matrices limits the small-molecule analysis because of the interferences in the low-mass region and reproducibility issues. To overcome these limitations, a surface-assisted laser desorption/ionization (SALDI), which utilizes nanostructured metallic surfaces, has been developed. Herein, a novel approach for SALDI–MS was proposed using nanoengineered gold shell with nanogaps on the silica core (SiO2@Au NGS), which is an emerging material due to its excellent heat-generating capabilities. The gold shell thickness was controlled by adjusting the concentration of gold precursor for the growth of gold nanoparticles. SALDI-MS measurements were performed on a layer formed by drop-casting a mixture of SiO2@Au NGS and analytes. At the optimized process, the gold shell thickness was observed to be 17.2 nm, which showed the highest absorbance. The ion desorption efficiency was confirmed with a survival yield upon fragmentation. Based on the enhanced SALDI capability, SiO2@Au NGS was utilized to detect various small molecules including amino acids, sugars, and flavonoids. The limits of detection, reproducibility, and salt tolerance of SiO2@Au NGS demonstrate its potential as an effective and reliable SALDI material for small-molecule analyses.

In this study, the use of recycled diatomaceous earth as the extraction phase in a the solid phase microextraction (SPME) technique for the determination of polycyclic aromatic hydrocarbons (PAHs) in river water samples, with separation/detection performed by gas chromatography-mass spectrometry (GC-MS), is proposed. The optimized extraction conditions are extraction time 70 min at 80 ºC with no addition of salt. The limits of quantification were close to 0.5 μg L-1 with RSD values lower than 25% (n = 3). The linear working range was 0.5 μg L-1 to 25 μg L-1 for all analytes. The method was applied to samples collected from the Itajaí River (Santa Catarina, Brazil) and the RSD values for repeatability and reproducibility were lower than 15% and 17%, respectively. The efficiency of the recycled diatomaceous earth fiber was compared with that of commercial fibers and good results were obtained, confirming that this is a promising option for use as the extraction phase in SPME.

In this study, we test the performance of a compact gas chromatograph with photoionization detector (GC-PID) and optimize the configuration to detect ambient (sub-ppb) levels of benzene, toluene, ethylbenzene, and xylene isomers (BTEX). The GC-PID system was designed to serve as a relatively inexpensive (~$10k) and field-deployable air toxic screening tool alternative to conventional benchtop GCs. The instrument uses ambient air as a carrier gas, and consists of a Tenax-GR trap preconcentrator, a gas sample valve, two capillary columns, and a photoionization detector (PID) with a small footprint and low power requirement. The performance of the GC-PID has been evaluated in terms of system linearity and sensitivity in field conditions. The BTEX-GC system demonstrated the capacity to detect BTEX at levels as high as 500 ppb with a linear calibration range of 0-100 ppb. A detection limit lower than 1 ppb was found for all BTEX compounds with a sampling volume of 1 L. No significant drift in the instrument was observed. A time-varying calibration technique was established that requires minimal equipment for field operations and optimizes the sampling procedure for field measurements. With an analysis time of less than 15 minutes, the compact GC-PID is ideal for field deployment of background and polluted atmospheres for near-real time measurements of BTEX. The results highlight the application of the compact and portable GC-PID for community monitoring and screening of air toxics.

Emerging pollutants as pharmaceuticals have been focusing international attention for few decades. Ciprofloxacin (CIP) is a common drug widely found in effluents from hospitals, industrial and different wastewater treatment plants, as well as rivers. In this work, the lab-scale 3D-BER system was established, and more than 90% of the antibiotic CIP removal from the Low C/N wastewater. Best results were obtained with current intensity, and different C/N ratio significantly improve the removal of CIP and nitrates, when the ideal conditions were; C/N = 1.5-3.5, pH =7.0-7.5, and I = 60 mA. The highest removal efficiency of CIP = 94.20 %, NO3--N= 95.53 % and total nitrogen (TN) = 84.27 %, respectively. In this novel system, the autotrophic-heterotrophic denitrifying bacteria played vital role for the removal of CIP and enhanced denitrification process. Thus, autotrophic denitrifying bacteria uses CO2 and H2 as carbon sources to reduce nitrates to N2. This system has the assortment and prosperous community revealed at the current intensity of 60 mA, and the analysis of bacterial community structure in effluent samples fluctuates under different condition of C/N ratios. According to the results of LC-MS/MS analysis, the intermediate products were proposed after efficient biodegradation of CIP. Microbial community on biodegrading was mostly found at phylum, and class level was dominantly responsible for the NO3--N and biodegradation of CIP. This work can provide some new insights towards the biodegradation of CIP and the efficient removal of nitrates from low C/N wastewater treatment by the novel 3D-BER system.

High-temperature cooking process like frying, baking, smoking, or drying can induce chemical transformations in conventional food ingredients, causing deteriorative modifications. These reactions, including hydrolytic, oxidative, and thermal changes, are a common occurrence and can result in alterations to the food's chemical composition. In this study, a combination of sucrose and histidine (Su-Hi) was transformed through a process of charring or pyrolysis. The GC-MS profiling study showed that when sucrose and histidine (Su-Hi) are exposed to high temperatures (≈240°C), they produce carbonyl and aromatic compounds including beta-D-Glucopyranose, 1,6-anhydro (10.11 %), 2-Butanone, 4,4-dimethoxy- (12.89 %), 2(1H)-Quinolinone-hydrazine (5.73%), Benzenamine (6.35%), 2,5-Pyrrolidinedione, 1-[(3,4-dimethylbenzoyl)oxy]- (5.82%), Benzene-(1-ethyl-1-propenyl) (5.62%), and 4-Pyridinamine-2,6-dimethyl (5.52%). The compounds mentioned have the ability to permeate the cell membrane and contribute to the development of cell death by necrosis in human immune cells. The evidence available suggests that a specific set of pyrolytic compounds may pose a risk to immune cells. This investigation reveals the complex relationship between high-temperature cooking-induced transformations, compound permeation inside the cells, and downstream cellular responses, emphasizing the significance of considering the broader health implications of food chemical contaminants.

A rapid, precise, accurate and low cost method for the determination of vitamin E (α-tocopherol) in cereal products and biscuits was developed. The uncertainty was calculated for the first time and the methods were performed in different cereal products and biscuits, characterized as “superfoods”. The limits of detection and quantification were calculated. Accuracy and precision were estimated using the certified reference material FAPAS T10112QC and the determined values were in good accordance with the certified values. The health claims according to the daily reference values for vitamin E were calculated and the results proved that the majority of the samples examined showed %daily value higher than 15%.

This study assesses the secondary metabolites, minerals, antimicrobial, antioxidant, and anticancer properties of Micromeria fruticosa plant different botanical parts (leaf, stem, root, flower) extracted with various solvents. The plant samples were sequentially obtained using different solvents (n-hexane, ethanol and water) through steeping. Then, each of the extracts was further analyzed by using gas chromatography–mass spectrometry (GC-MS). Moreover, the extracts were bio-assayed to test their antioxidant, antibacterial, and anti-cancer activities. Quali-quantitative analysis of M. fruticosa crude extracts revealed the occurrence of 27 secondary metabolites were identified including mainly monoterpenes, sesquterpenes, and fatty acids, with varying quantities. Some of the major bioactive compounds included, Menthone (5.42-30.05%), Oleamide (3.40-32.20%), Pulegone (10.66-64.1%), and Menthol (3.61-100.0%), which were detected mostly in all plant parts with significant quantities. Several antioxidant minerals, mainly, Fe, Zn, and Mn, were detected with the highest amounts in the Micromeria water extracts. Results from antimicrobial assays showed that the water extract of leaves exhibited the highest DPPH scavenging activity (89.73%) followed by the water extract of flowers (80.07%) at a concentration of 100 μg/mL. The water extract of stems showed greater antimicrobial activity against all the tested gram negative and positive bacteria (Methicillin-resistant Staphylococcus aureus, Staphylococcus aureus, Escherichia coli, and Shigella sonnie). The leaves ethanolic and stem aqueous extracts had a strong antimicrobial activity against E. coli. and C. albicans. Flower aqueous extract demonstrated the highest cytostatic effect on the colon cell line by reducing viability up to 30.4%, followed by the leaf ethanol extract with 38.6% cell viability reduction at 1000 µg/mL. In conclusion, extraction solvents influenced the recovery of phytocompounds and the highest pharmacological activities of the different extracts could be correlated to the presence of additional bioactive compounds. Our results suggest that M. fruticosa plant is a promising source of natural products with antioxidant, anti-microbial and anti-cancer properties for potential nutraceutical, therapeutic, and functional food applications. , , , , , ,

Fructus Amomi (FA) is usually regarded as the dried ripe fruits of Amomum villosum Lour. (FAL) or Amomum villosum Lour. var. xanthioides T. L.Wu et Senjenis (FALX) However, FAL, which always has a much higher price because of its better quality, is confused with FALX in the market. As volatile oil is the main constituent of FA, a strategy of chromatography-mass spectrometry (GC-MS) and chemometric approches was applied to compare the chemical composition of FAL and FALX. The results showed that the oil yield of FAL was significantly higher than that of FALX. Total ion chromatograph (TIC) showed that cis-nerolidol existed only in FALX. Bornyl acetate and camphor, could be considered as the most important ones in FAL and FALX respectively. Moreover, hierarchical cluster analysis (HCA) and principal component analysis (PCA) successfully distinguished the chemical constitutes of the volatile oils in FAL and FALX. Additionally, bornyl acetate, α-cadinol, linalool, β-myrcene, camphor, d-limonene, terpinolene and endo-borneol were selected as the potential markers for discriminating FAL and FALX by partial least squares discrimination analysis (PLS-DA). In conclusion, this present study first developed a scientific approach to separate FAL and FALX based on volatile oils by GC-MS combined with chemometric techniques.

In the process of oil and gas development and production, when the flow rate in the wellbore is large, the materials underground will be eroded, causing the operation to be unable to proceed smoothly and reducing the efficiency of oil and gas production. Therefore, optimizing the anti-erosion coating under high-speed flow conditions in wellbore is a very interesting thing. It can greatly improve operational efficiency. In this paper, laser cladding was used to prepare the new coating used in the PDC drill bit. Then, the effects of tungsten carbide and multi-layer graphene on the microstructure and properties of the tungsten carbide coating were studied. The research results indicate that, for new coatings, 60% tungsten carbide and 0.3% graphene are the optimal ratios. After adding WC, the hardness has significantly improved. However, when the WC content further increases more than 30%, the increase in hardness is relatively small. In addition, when the content of graphene is more than 0.3%, the branched structure became thicker, and not only the segregation of Cr, Si and W became very obvious again, but also the segregation of Fe occurred at the Ni enrichment site. The research results contribute to improving oil and gas production and operational efficiency under high-speed fluid flow conditions in the wellbore.

The profile of secondary metabolites occurring in apple cuticular layer is not only characteristic for particular apple cultivar, but also dynamically reflects various external factors in growing environment. In this study, the possibility to authenticate apple samples based on analysis of their cuticular layer extracts was investigated. Ultra-high-performance liquid chromatography coupled to high resolution tandem mass spectrometry (UHPLC-HRMS/MS) was employed for obtaining metabolomic fingerprints. In total, 274 authentic apple samples, four cultivars harvested within the seasons 2020 to 2022 in the Czech Republic and Poland were analysed. The generated complex data processed by univariate and multivariate statistical methods enabled to build classification models for discrimination of apple cultivars as well as their geographical origin. The models showed very good performance in differentiation of Czech and Polish samples for three of four cultivars: ‘Gala’, ‘Golden Delicious’ and ‘Idared’, moreover, the validity of the models was verified over harvest seasons. The diagnostic markers, besides metabolites of triterpene biosynthetic pathway, mainly represented wax esters. ‘Jonagold’, which is known to be susceptible to mutations, was the only cultivar for which the unambiguous classification of geographical origin was not possible.

The present work describes the optimization and validation of a highly selective and sensitive analytical method using solid phase extraction and liquid chromatography tandem mass spectrometry (SPE LC-MS/MS) for the determination of some frequently prescribed pharmaceuticals in urban wastewater received and treated by Sharjah sewage treatment plant (STP). The extraction efficiency of different SPE cartridges was tested and the simultaneous extraction of pharmaceuticals was successfully accomplished using hydrophilic-lipophilic-balanced reversed phase Waters^® Oasis HLB cartridge (200 mg/ 6 mL) at pH 3. The analytes were separated on an Aquity BEH C₁₈ column (1.7 µm, 2.1 mm x 150 mm) using gradient elution and the mass spectrometric analysis were performed in multiple reactions monitoring (MRM) selecting two precursor ions to produce ion transition for each pharmaceutical using positive electrospray ionization (+ESI) mode. The correlation coefficient values in the linear calibration plot for each target compound exceeded 0.99 and the recovery percentages of the investigated pharmaceuticals were more than 84%. Limit of detection (LOD) varied between 0.1-1.5 ng/L and limit of quantification (LOQ) was 0.3-5 ng/L for all analytes. The precision of the method was calculated as the relative standard deviation (RSD%) of replicate measurements and was found to be in the ranges of 2.2% to 7.7% and 2.2% to 8.6% for inter and intra-day analysis, respectively. All of the obtained validation parameters satisfied the requirements and guidelines of analytical method validation.

To determine promethazine (PMZ) and its metabolites promethazine sulfoxide (PMZSO) and monodesmethyl-promethazine (Nor1PMZ) in swine muscle, fat, kidney, and liver, a sample preparation and high-performance liquid chromatography-tandem mass spectrometry (LC-MS/MS) analysis method were established and validated. The sample was extracted with 0.1% formic acid-acetonitrile, and the extract was purified with acetonitrile-saturated n-hexane. After concentration by rotary evaporation, the extract was re-dissolved in 0.1% formic acid-water and acetonitrile (80:20, v/v). The HPLC-MS/MS column used was a Waters Symmetry C18 (100 mm × 2.1 mm i.d., 3.5 μm), with 0.1% formic acid-water and acetonitrile as the mobile phase, and the target compounds were determined by positive ion scan and multiple reaction monitoring. PMZ and Nor1PMZ were quantified with deuterated promethazine (PMZ-d6) as the internal standard, while PMZSO was quantified by external standard method. The limits of detection (LOD) and limits of quantification (LOQ) of PMZ and PMZSO in muscle, liver, and kidney spiked samples were 0.05 μg/kg and 0.1 μg/kg, respectively, while those of Nor1PMZ were 0.1 μg/kg and 0.5 μg/kg, respectively. The LOD and LOQ of analytes in fat spiked sample were 0.05 μg/kg and 0.1 μg/kg, respectively. The sensitivity of this method reaches or exceeds its presented in previous reports. The analytes PMZ and PMZSO showed good linearity within the range of 0.1 μg/kg to 50 μg/kg, while Nor1PMZ showed good linearity within the range of 0.5 μg/kg to 50 μg/kg, with correlation coefficients (r) greater than 0.99. The recoveries of the target compounds in the sam-ples were between 81.73% and 107.17%, and the precision ranged from 1.78% to 10.47%. This study developed for the first time an HPLC-MS/MS method for the determination of PMZ and its metabolites PMZSO and Nor1PMZ in four swine edible tissues, comprehensively covered target tissues of monitoring object, which is applicable for monitoring veterinary drug residues in ani-mal-derived foods and ensuring food safety.

The interest in lipid composition profiling is significantly increasing as research reveals the immense importance of lipids in medicine, plant science, food and agriculture. However, lipidomic analysis requires high-end specialty equipment. We used two-dimensional thin-layer chromatography (2D TLC) as a readily available, low-cost tool for basic lipidomic profiling of lipid classes in algal samples as model: Chlamydomonas reinhardtii, Auxenochlorella protothecoides, and Euglena gracilis. Algal lipid extracts were separated on a 2D-TLC plate, and TLC analysis was followed by scraping individual TLC spots off the plate, and a subsequent liquid chromatography separation and tandem mass spectrometry (LC-MS/MS) analysis. For comparison, crude lipid extracts were also injected directly to the LC-MS/MS system. Lipid class annotation was achieved by a combination of accurate mass, retention time information, neutral loss and fragment ion analysis by MS2Analyzer, and by matching spectra to LipidBlast MS/MS library. Overall, we were able to identify 15 lipid classes, and to adequately profile the lipid classes in all three organisms. This TLC method is thus suggested as an accessible tool for lipid class profiling of algal, plant, and food lipids, alike, when a rapid and simple analysis is required, e.g., for screening purposes.

The poly lactic acid (PLA) is one of the most used bio-derived thermoplastic polymers in 3D and 4D printing applications. The determination of PLA surface properties is of capital importance in 3D/4D printing technology. (1) Background: The surface thermodynamic properties of PLA polymer were determined by using the inverse gas chromatography (IGC) technique at infinite dilution. The determination of the retention volume of polar and non-polar molecules adsorbed on the PLA particles filling the column allowed us to obtain the dispersive, polar, and Lewis’s acid-base surface properties at different temperatures from 40 °C to 100 °C. (2) Methods: the applied surface method was based on our recent model that used the London dispersion equation and the new chromatographic parameter function of the deformation polarizability and the harmonic mean of the ionization energies of the PLA polymer and organic molecules. (3) Results: The application of this new method led to the determination of the dispersive and polar free surface energy of adsorption of molecules on the polymeric material, as well as the glass transition and the Lewis acid-base constants. (4) Conclusions: four interval temperatures were distinguished showing four zones of the variations of the surface properties of PLA as a function of the temperature before and after the glass transition.

Stable-isotope dimethyl labeling is a highly reactive and cost-effective derivatization procedure that could be utilized in proteomics analysis. In this study, a liquid chromatography-tandem mass spectrometry in multiple reaction monitoring mode (LC-MS-MRM) platform for the quantification of kiwi allergens was first developed using this strategy. Three signature peptides for target allergens Act d 1, Act d 5, and Act d 11 were determined and were derivatized with normal and deuterated formaldehyde as external calibrants and internal standards, respectively. The results showed that sample preparation with the phenol method provided comprehensive protein populations. Recoveries at four different levels ranging from 72.5–109.3% were achieved for the H-labeled signature peptides of Act d 1 (SPA1-H) and Act d 5 (SPA5-H) with precision ranging from 1.86–9.92%. The limit of quantification (LOQ) was set at 8 pg mL–1 for SPA1-H and at 4 ng mL–1 for SPA5-H. The developed procedure was utilized to analyze seven kinds of hand-made kiwi foods containing 0.0175–0.0515 mg g–1 of Act d 1 and 0.0252–0.0556 mg g–1 of Act d 5. This study extended the applicability of stable-isotope dimethyl labeling to the economical and precise determination of food allergens and peptides.

From their discovery in 2002, BRAF mutations have been identified as clear drivers of oncogenesis in several cancer types. Currently, their incidence rate is nearly 7% of all solid tumors with BRAF V600E constituting approximately 90% of these diagnoses [1]. In melanoma, thyroid cancer, and histiocytic neoplasms, BRAF hotspot mutations are found at a rate of about 50%, while in lung and colorectal cancers they range from 3 to 10% of reported cases [2-5]. Though present in other malignancies such as breast and ovarian cancers, they constitute a small portion of diagnoses (<1%). Given their frequency along with advancements in screening technologies, various methods are used for the detection of BRAF-mutant cancers. Among these are targeted next-generation sequencing (NGS) on tumor tissue or circulating tumor DNA (ctDNA) and immunohistochemistry (IHC)-based assays. With advancements in detection technologies, several approaches have been taken for the treatment of BRAF mutant cancers. In this review we retrace the milestones that led to the clinical development of targeted therapies currently available for these tumors.

Adenosine is a multifunctional nucleoside with several roles across various levels in organisms. Beyond its intracellular involvement in cellular metabolism, extracellular adenosine potently influences both physiological and pathological processes. In relation to its blood level, adenosine impacts the cardiovascular system, such as heart beating rate and vasodilation. To exploit the adenosine levels in the blood, we employed the liquid chromatography method coupled with mass spectrometry (LC-MS). Immediately after the collection, a blood sample mixed with acetonitrile solution that is either enriched with 13C-labeled adenosine or a newly generated mixture is transferred into the tubes containing the defined amount of 13C-labeled adenosine. The 13C-enriched isotopic adenosine is used as an internal standard, allowing for more accurate quantification of adenosine. This novel protocol for LC-MS-based estimation of adenosine delivers a rapid, highly sensitive, and reproducible means for quantitative estimation of total adenosine in blood. The method also allows quantification of a few catabolites of adenosine, i.e., inosine, hypoxanthine, and xanthine. This advancement provides the analytical tool that has the potential to enhance our understanding of adenosine's systemic impact and pave the way for further investigations into its intricate regulatory mechanisms.

The spread of SARS-CoV-2 variants of concern (VOCs), is of great importance to the whole community, since their genetic changes may increase transmissibility, disease severity and reduce effectiveness of vaccines. Moreover, these changes may lead to failure of diagnostic measures, thus variant-specific diagnostic methods are essential. To date, genetic sequencing is the gold standard method to discriminate between variants, however it is time consuming (several days) and expensive. Therefore, the development of rapid diagnostic methods for SARS-CoV-2 in accordance with its genetic modification is of great importance. In this study, we introduce a Mass-Spectrometry (MS)-based methodology for the diagnosis of SARS-CoV-2 in clinical specimens, a methodology which enables universal identification, alongside with variant-specific discrimination. The universal identification of SARS-CoV-2 is based on conserved markers shared by all variants, while the identification of the specific variant relies on variant-specific markers. Determining a specific set of peptides for a given variant consists of a multistep procedure, starting with in-silico search for variant-specific tryptic peptides, followed by tryptic digest of a cell-cultured SARS-CoV-2 variant and identification of these markers by HR-LC-MS/MS analysis. As a proof of concept, this approach was demonstrated for four representative VOCs, in comparison with the wild-type Wuhan reference strain. For each variant, at least two unique markers, derived mainly from the spike (S) and nucleocapsid (N) viral proteins, were identified. This methodology is specific, rapid, easy to perform and inexpensive, therefore can be applied as a general diagnostic tool of pathogenic variants.

A PLS-based quality prediction method is proposed for batch processes using two-dimensional extended windows. To realize the adoption of information in the direction of sampling time and batch, a new definition region of support (ROS), k-i-back-extended region of support (KIBROS), is proposed to establish the extended window, which including the data of the previous sampling times in the same batch, the data of the same sampling time in the historical batches, the data of the previous sampling times in the historical batches and the data of the later sampling times in the historical batches. According to these regions of support, extended windows are established, and different models are proposed based on the extended windows for batch processes quality prediction. Further, using a typical batch process as an example, the injection molding process, the proposed quality prediction method is experimentally verified, proving that the proposed methods have higher prediction accuracy than the traditional method and the prediction stability is also improved.

The aquaculture industry has become a sustainable provider of food to humans. Remaining challenges include disease issues, as well as ethical concerns for discomfort and stress among farmed fish. There is a need for reliable biomarkers to monitor welfare in fish, and the stress hormone cortisol has been suggested as a good candidate. This study presents a novel method for measurement of cortisol in fish feces based on enzymatic hydrolysis, liquid-liquid extraction, derivatization, and finally instrumental analysis by liquid chromatography coupled with tandem mass spectrometry. Hydrolysis and extraction conditions were optimized. Cortisol appeared to be mostly conjugated to sulfate and less conjugated to glucuronic acid in the studied samples of feces from farmed Atlantic salmon. The method was suitable for quantification of cortisol after enzymatic deconjugation by either combined glucuronidase and sulfatase activity, or by glucuronidase activity alone. The limit of detection was 0.15 ng/g and the limit of quantification was 0.34 ng/g, and the method was linear (R2>0.997) up to 380 ng/g, for measurement of cortisol in wet feces. Method repeatability and intermediate precision were acceptable, both with a CV of 11%. Stress level was high in fish released into seawater, and significantly reduced after eight days.

A sensitive and robust liquid chromatography-tandem mass spectrometric (LC-MS/MS) method was developed and validated for the determination of nimbolide in mouse serum. Exemestane was used as the internal standard (IS). Here, we employed acetonitrile-based protein precipitation (PPT) for serum sample preparation, and performed chromatographic separation using an ODS Hypersil C18 column (100×2.1 mm, 5µm) with gradient elution (0.1% formic acid in water vs 100% acetonitrile). The run time was 6 min. Instrumental analysis was performed by electrospray ionization tandem mass spectrometry (ESI-MS/MS) in the multiple-reaction monitoring (MRM) under positive mode. A good linear calibration was achieved in the 5–1000 ng/ml range. The intra- and inter-day precisions for nimbolide were ≤ 12.6% and ≤ 13.9 % respectively. Intra-day accuracy ranged from 96.9% – 109.3% while inter-day accuracy ranged from 94.3% – 110.2%. The matrix effect of nimbolide, detected but consistent at low and high concentrations, do not affect linearity of standard curve. In conclusion, we have developed and validated a sensitive analytical method for determination of a novel natural compound nimbolide in mouse serum and it has been successfully applied to our preclinical study in investigating the pharmacokinetic properties of nimbolide, which could greatly facilitate the preclinical development of the promising lead compound for anticancer therapy.

The Asian world is home to a multitude of venomous and dangerous snakes, which are attributed to various medical effects used in the preparation of traditional snake tinctures and alcoholics, like the Japanese snake wine, named Habushu. The aim of this work was to perform the first quantitative proteomic analysis of the Protobothrops flavoviridis pit viper venom. Accordingly, the venom was analyzed by complimentary bottom-up and top-down mass spectrometry techniques. The mass spectrometry-based snake venomics approach revealed that more than half of the venom is composed of different phospholipases A2 (PLA2). The combination with an intact mass profiling led to the identification of the three main Habu PLA2s. Furthermore, nearly one-third of the total venom consists of snake venom metalloproteinases and disintegrins, and several minor represented toxins families were detected: CTL, CRISP, svSP, LAAO, PDE and 5’-nucleotidase. Finally, the venom of P. flavoviridis contains certain bradykinin-potentiating peptides and related peptides, like the svMP inhibitors pEKW, pEQW, pEEW and pENW. In preliminary MTT cytotoxicity assays the highest cancerous-cytotoxicity of the crude venom was measured against human neuroblastoma SH-SY5Y cells and shows in some fractions disintegrin-like effects.

The commercial cultivation of microalgae began in the 1960s and Chlorella was one of the first target organisms. The species has long been considered a potential source of renewable energy, an alternative for phytoremediation, and more recently, as a growth and immune stimulant. However, Chlorella vulgaris, which is one of the most studied microalga, has never been comprehensively profiled chemically. In the present study, comprehensive profiling of the Chlorella vulgaris metabolome grown under normal culture conditions was carried out, employing tandem LC-MS/MS to profile the ethanolic extract and GC-MS for fatty acid analysis. The fatty acid profile of C. vulgaris was shown to be rich in omega-6, -7, -9, and -13 fatty acids, with omega-6 being the highest, representing more than sixty percent (>60%) of the total fatty acids. This is a clear indication that this species of Chlorella could serve as a good source of nutrition when incorporated in diets. The profile also showed that the main fatty acid composition was that of C₁₆-C₁₈ (>92%), suggesting that it might be a potential candidate for biodiesel production. LC-MS/MS analysis revealed carotenoid constituents comprising violaxanthin, neoxanthin, lutein, β-carotene, vulgaxanthin I, astaxanthin, and antheraxanthin, along with other pigments such as the chlorophylls. In addition to these, amino acids, vitamins, and simple sugars were also profiled, and through mass spectrometry-based molecular networking, 48 phospholipids were putatively identified.

Soybean, maize and bean are crops of great economic importance, but in the last years suffered with infestations of the caterpillar Helicoverpa armigera, being the main problem the resistance of this pest to most pesticides. Avermectin emamectin benzoate was recently released to control this pest. Other avermectins, like abamectin, doramectin, eprinomectin and ivermectin are used in large scale because they potent acaricidal, anthelmintic, and insecticidal activities. Thus, a simple and fast method for the determination of avermectins in these crops based on a quick, easy, cheap, effective, rugged and safe (QuEChERS) extraction procedure and ultra-high performance liquid chromatography with tandem mass spectrometry (UHPLC-MS/MS) analysis was developed and validated. For extraction, water followed by acetonitrile:isopropanol and a partition step with salts was stablished. With the clean-up step using activated EMR-Lipid, limits of detection of 1.2 μg kg-1 for abamectin, doramectin, emamectin benzoate and ivermectin, and of 2.4 μg kg-1 for eprinomectin were achieved. Accuracy and precision evaluated at low levels presented satisfactory results. The method was successfully applied in commercial samples and is a good alternative for routine analysis.

Subacute rumen acidosis (SARA) is a prevalent issue in intensive livestock farming, particularly associated with high-concentrate diets. This study investigates the prevalence and impact of SARA in Greek dairy sheep farming and explores the use of computerized rumen colorimetry as a management and diagnostic tool for SARA in dairy sheep farms. Forty-two dairy sheep flocks were monitored regularly for rumen pH, milk composition, and milk yield over an approximately 9-month milking period. Computerized Rumen Mucosal Colorimetry was applied to 280 culled, aged ewes from these farms, with rumen wall samples taken for histological examination. SARA cases were identified in 19 farms (45%, n=48). Farms with SARA cases had lower milk fat levels, although milk yield was higher in these farms, while milk protein levels did not differ based on the SARA status of the farms. In culled ewes, rumen color was significantly associated with the farm's SARA status. Additionally, ewes from farms with more SARA cases exhibited increased thickness in the ruminal epithelium layers, particularly in the non-keratinized and total epithelium layers. In conclusion, SARA is a common disorder in the Greek dairy sheep industry, lowering the fat content of milk. The study suggests that computerized rumen epithelium colorimetry in aged culled ewes shows promise as a diagnostic tool for SARA in dairy sheep farms.

Plant cells' ability to withstand abiotic stress is strongly linked to modifications in their mechanical characteristics. Nevertheless, the lack of a workable method for consistently tracking plant cell mechanical properties severely restricts our comprehension of the mechanical alterations in plant cells under stress. With Polyethylene Glycol (PEG6000), we created a drought-like environment, and we used the Double Resonator Piezoelectric Cytometry (DRPC) method to dynamically and non-invasively track changes in the stress (ΔS) created and viscoelasticity (storage modulus G' and loss modulus G") of protoplasts and suspension cells of rice during drought stress. The findings demonstrate that, rice suspension cells and protoplasts react mechanically differently to 5%–15% PEG6000 stress, implying distinct resistance mechanisms. However, neither of them can withstand 25% PEG6000 stress, they respond mechanically similarly to 25% PEG6000 stress. The results of DRPC are further corroborated by the morphological alterations of rice cells and protoplasts observed under an optical microscope. To sum up, the DRPC technique functions as a precise cellular mechanical sensor and offers novel research tools for the evaluation of plant cell adversity and differentiating between the mechanical reactions of cells and protoplasts under abiotic stress.

Astaxanthin (ATX) is a carotenoid nutraceutical with a poor bioavailability due to its high lipophilicity. We tested a new tailored nano-droplet capable of solubilizing ATX in an oil-in-water micro-environment (LDS-ATX, manufactured by Lyotropic Delivery Systems (LDS)), for its capacity to improve ATX pharmacokinetic profile and anti-oxidant efficacy. We used liquid chromatography tandem mass spectrometry (LC-MS/MS) to compare the pharmacokinetic profile of ATX and LDS-ATX and protein carbonylation and lipid peroxidation assays to compare their basal and lipopolysaccharide (LPS)-induced oxidative damage. Our results show that only LPS-induced oxidative damage was corrected by ATX and LDS-ATX. While in the liver and muscle LDS-ATX was more efficacious than ATX in attenuating oxidative damage to both proteins and lipids, only oxidative damage to lipids was preferably corrected by LDS-ATX in the brain. These results strongly suggest improvement of ATX bioavailability and efficacy by the LDS-ATX nano-formulation.

The literature was scoped to help place mass spectrometric (MS) platforms in the spotlight of the life sciences, as a tool of OMICS and OMICS 2.0 technologies. Moreover, today’s appliances are so handy, that they literally place a whole lab on a single chip. Methods of OMICS (and the most recently developed term OMICS 2.0) are tackled, having in mind their aptness for educational purposes, as well as their feasibility. This same topic was highlighted in many reviews that have been periodically published. The author’s initial interest was the forensic application of MS, but since these interests changed, terms such as “biosensors” were also examined, so the review included means of discovery of efficient biomarkers and clinical therapeutic targets. Aside from simply reviewing the research status and the future perspectives, this article tackles terms such as Society 5.0 and OMICS 2.0. However, within the framework of this review, physical chemistry, bioinformatics, or specific software solutions were not specifically studied. Since the topic of generating permanent collections of digital content for retrospective analysis was also reviewed, the need for loads of data – cloud storage was discussed in the context of MS. These large quantities of data are easier to operate with if generated by MS, rather than by any other commercially available assay. In this manner, the review has strengthened an in-depth understanding of the applications of MS.

Purpose of publication: - Preparation of bibliometric data exported from the Scilit platform on energy efficiency and conservation for further analysis to identify relevant research topics. - To identify potential issues in the processing of data exported from the Scilit platform. - Providing colleagues with the opportunity to use the prepared data and examples of their analysis for independent research on topical issues of energy efficiency and energy conservation using materials provided by the Scilit platform. Research Materials: Files in CSV and RIS formats exported from Scilit for the query "energy conservation OR efficiency" in Common Fields [Title, Abstract, Keyword], using filters: Content Type → Journal Article; Year→2021-2023; Subject → Industrial Engineering (29.8K), Energy and Fuel Technology (9.8K), Manufacturing Engineering (9.2K). A total of 30K records sorted by their relevance (10K for each year) were exported. Data are current as of 14-03-2024. Methods: Preprocessing of title, annotation, and keyword field texts using lemmatization dictionaries collected on GitHub, removal of keywords taken from GATE and spaCy, and "manual" editing. Using VOSviewer to analyze publication topics by clustering keywords based on their co-occurrence. Using Scimago Graphica to build bubble diagrams.Application of the GSDMM algorithm for clustering bibliometric records by title and annotation texts. Creation of a dictionary for this algorithm using the keyword field.Use of the Carrot2 demo version and the NMF algorithm for a more detailed analysis of the topics of the record clusters obtained from GSDMM. Results: are presented in the form of initial and interim tables and graphs obtained in the course of this study. The full tables are provided as references to the attached materials. Supplementary material for this preprint on figshare: Chigarev, Boris (2024). Supplementary material for preprint "Analyzing the Possibilities of Using the Scilit Platform to Identify Current Energy Efficiency and Conservation Issues". figshare. Dataset. https://doi.org/10.6084/m9.figshare.25574058.v1

The study of exogenous metabolites of algae-bacterial communities in the laboratory accumulative culture obtained from natural river water was done using gas chromatography-mass spectrometry. Exometabolites of the algae-bacterial community (including microalgae and cyanobacteria) in the culture medium were represented by saturated, unsaturated, and aromatic hydrocarbons, carboxylic acids, phenolic, and terpene compounds and their derivatives. Possible biological activities of the discovered exometabolites are considered. The study has demonstrated that an increase in the number of main groups of microorganisms, along with changes in the composition of algae and cyanobacteria, are responsible for the increase in the composition and concentration of metabolites in the microecosystem's culture medium after one month of cultivation. The presence of octacosane in high concentration (0.0603 mg/l; 23.78% of the total content of low molecular weight organic compounds) by the end of exposure accumulative culture is associated with the strong development of the cyanobacterium Gloeocapsa sp. in the presence of diatom algae of the genus Navicula and green algae of the genera Chlorella and Scenedesmus. Due to the need to comprehend the ecological and biochemical mechanisms of the formation and functioning of algae-bacterial communities, as well as to predict potential paths of transformation and evolution of aquatic ecosystems, the specificity of exometabolite complexes of algae and microorganisms, as well as their allelopathic and other biochemical interactions in freshwater ecosystems, requires further serious study.

In this research, we utilize density functional theory (DFT) to study and investigate the adsorption process of methanol on three unique two-dimensional nanomaterials, namely BN, Graphene, and AlN. Eight sites for BN, AlN, and six sites for graphene were considered to reach full structural optimization. By conducting comprehensive simulations and analyses, we discovered diverse adsorption configurations and energy levels, which indicate different interaction strengths between methanol and the three 2D nanomaterials. Remarkably, AlN exhibits superior adsorption capabilities when compared to Graphene and BN which can be explained by attributable to the nature of charge transfer between the adsorbate and the adsorbent. For methanol adsorption on AlN, the strongest adsorption energy was (-0.5532 eV), and the amount of charge transferred from methanol to AlN was found to be (+0.075). For BN, the strongest adsorption energy was (-0.1351 eV), and the amount of charge transferred from methanol to BN was (+0.022). The density of states results indicated that the bandgap decreased, with a shift to the right. In contrast, for methanol adsorption on graphene, the strongest adsorption energy was found to be (-0.073 eV), and the amount of charge transferred from methanol to graphene was (+0.004). The density of states results showed no change in the bandgap. Our findings underscore the superiority of AlN’s potential over BN and Graphene for applications requiring efficient methanol adsorption, such as gas separation and storage technologies. This study emphasizes the superiority of AlN over Graphene and BN for tasks that necessitate effective methanol adsorption.

Untargeted and targeted approaches are the traditional metabolomics workflows acquired for a wider understanding of the metabolome under focus. Both approaches have their strengths and weaknesses. The untargeted, for example, is maximizing the detection and accurate identification of thousands of metabolites, while the targeted is maximizing the linear dynamic range and quantification sensitivity. These workflows, however, are acquired separately, so researchers compromise either a low-accuracy overview of total molecular changes (i.e., untargeted analysis) or a detailed yet blinkered snapshot of a selected group of metabolites (i.e., targeted analysis) by selecting one of the workflows over the other. In this review, we present a novel single injection simultaneous quantitation and discovery (SQUAD) metabolomics that combines targeted and untargeted workflows. It is used to identify and accurately quantify a targeted set of metabolites. It also allows data retro-mining to look for global metabolic changes that were not part of the original focus. This offers a way to strike the balance between targeted and untargeted approaches in one single experiment and address the two’s limitations. This simultaneous acquisition of hypothesis-led and discovery-led datasets allows scientists to gain more knowledge about biological systems in a single experiment.

Surface Plasmon Resonance (SPR) based sensors have the advantage of being label-free, enzyme-free and real-time. However, their spreading in multidisciplinary research is still limited and almost confined to prism-coupled devices. Plasmonic gratings, combined with a simple and cost-effective instrumentation, have been poorly developed compared to prism-coupled system mainly due to their lower sensitivity. Here we describe the optimization and signal enhancement of a sensing platform based on phase-interrogation method, which entails the exploitation of a nanostructured sensor. This technique is particularly suitable for integration of the plasmonic sensor in a lab-on-a-chip platform and can be used in a microfluidic circuit to ease the sensing procedures and limit the injected volume. The careful optimization of most suitable experimental parameters by numerical simulations leads to a 30 to 50% enhancement of SPR response, opening new possibilities for applications in the biomedical research field while maintaining the ease and versatility of the configuration.

Among the many neglected underutilized species, tuberous Andean root crops like the ahipas (Pachyrhizus ahipa) constitute a promising alternative for increasing diversity in nutrient sources and food security at a regional level. In this study, we present the content of some functional compounds in tuberous roots from several ahipa accessions and the progenies of the interspecific hybrid X207 (P. ahipa × P. tuberosus). A significant objective was to determine protein and free amino acids in the roots to evaluate their food quality as protein supply. The interspecific hybrids have been found to possess the root quality to provide the crop with a higher dry matter content. The high dry matter content of the P. tuberosus Chuin materials is retained in the root quality of the hybrids. Food functional components like carbohydrates, organic acids, and proteins were determined in several ahipa accessions and a stable (non-segregating) progeny of the interspecific hybrid, X207. The X207 roots showed a significantly higher dry matter content and a lower content in soluble sugars, but no significant differences were found in starch content or organic acids compared to the ahipa accessions. About the root mineral contents, Fe and Mn concentrations in X207 were significantly raised compared to the average of ahipa accessions. Among the ahipa and the hybrid, no prominent differences in protein content or protein amino acids were found, being both partially defective in providing sufficient daily intake of some essential amino acids. Root weight, a central component of root yield, was significantly higher in X207, but thorough field studies are required to substantiate the hybrid’s superior yield performance..

Saffron, renowned for its aroma and flavor, is susceptible to adulteration due to its high value and demand. Current detection methods, including ISO standards, often fail to identify specific adulterants such as safflower or turmeric up to 20% (w/w). Therefore, the quest continues for robust screening methods using advanced techniques to tackle this persistent challenge in safeguarding saffron quality and authenticity. Advanced techniques like Time of Flight Secondary Ion Mass Spectrometry (TOF-SIMS), with its molecular specificity and high sensitivity, offer promising solutions. Samples of pure saffron and saffron adulterated with safflower and turmeric at three levels of inclusion (5%, 10%, and 20%) were analyzed without prior treatment. Spectral analysis revealed distinct signatures for pure saffron, safflower, and turmeric. Through Principal Component Analysis (PCA), TOF-SIMS effectively discriminated between pure saffron and saffron adulterated with turmeric and safflower at different inclusion levels. The variation between the groups is attributed to the characteristic peaks of safflower and the amino group peaks and mineral peaks of saffron. Additionally, a study was conducted to demonstrate that semi-quantification of the level of safflower inclusion can be achieved from the normalized values of its characteristic peaks in the saffron matrix.

Natural gas is an important energy source among various fossil fuels. However, natural gas typically contains a significant amount of water vapor, which can pose challenges in its usage. Therefore, the process of removing water vapor from natural gas, known as gas dehydration, is crucial in the gas industry. The presence of water vapor in the gas supply can lead to the formation of hydrates, which can cause issues such as blockages in pipelines. To tackle this problem effectively, gas dehydration makes use of Tri ethylene glycol (TEG) as a drying agent. TEG works by selectively absorbing water vapor from the natural gas flow, thereby significantly reducing its moisture content.In the gas dehydration process, wet gas is treated by using lean glycol in an absorber, where the water vapor is removed. The resulting rich glycol is then recovered and recycled for further use. In this study, we explore the possibility of replacing nitrogen with dry natural gas in the re-generator of the glycol dehydration system. The aim is to evaluate the feasibility and effectiveness of this alternative approach. To assess the performance of both techniques, we employed HYSYS modeling and simulation. Through this analysis, we compared the capital and utility expenses associated with each method while ensuring that the glycol purity requirements remained unchanged. By examining the results obtained from the simulations, we can gain insights into the economic viability and efficiency of utilizing dry natural gas in the re-generator stage of the glycol dehydration process.In addition to the primary purpose of removing water vapor, the wet gas obtained from the stripping mechanisms in the glycol dehydration process can serve additional functions. It can be utilized to power steam pumps and compressors, thereby maximizing energy efficiency within the system. Alternatively, the wet gas can be recycled back into the process for further treatment. To develop a comprehensive understanding of the entire mechanism, we constructed a model based on the actual flow diagram. This model takes into account the various components and processes involved in the glycol dehydration system, including the stripping mechanisms and their connection to other equipment. By analyzing the data and outcomes generated by this model, we can derive valuable insights. These findings can be utilized to optimize the heat and material balance within the plant, ensuring efficient operation and potentially leading to the design of an improved system in terms of energy consumption and overall performance

Among other fossil fuels, natural gas is a major energy source. It is generally created saturated with water vapor. Dehydration of natural gas is vital in the gas business to remove water vapor from the gas supply, which may cause hydrate development in pipes. Gas dehydration employs Tri ethylene glycol (TEG) to remove water vapor from natural gas flow. The wet gas is dehydrated with lean glycol in an absorber, and the rich glycol is recovered and reused. This work investigates the use of dry natural gas instead of nitrogen in the glycol dehydration re-generator, and compares the results using HYSYS modeling and simulation. The two techniques were compared for capital and utility expenses, while maintaining the identical glycol purity criteria. The wet gas from the stripping mechanisms may also be utilized to run steam pumps and compressors or recycled. The model is based on the real mechanism flow diagram. Finally, the findings of this model might be used to design a new heat and material balance for the plant.

Chemical analysis of the organic components in beers has applications to quality control, authenticity and improvements to the flavor characteristics and brewing process. This study aims to show the complementary nature of two instrumental techniques which in combination can identify and quantify the majority of organic components in a beer sample. Nuclear Magnetic Resonance (NMR) was used to provide concentrations of twenty five different organic compounds including alcohols, organic acids, carbohydrates, and amino acids. Calorie content was also estimated for the samples. NMR data for ethanol concentrations were validated by comparison to a Fourier Transform Infrared Spectrometry (FTIR) method. Headspace Solid-Phase Microextraction (SPME) Gas Chromatography Mass Spectrometry (GCMS) was used to identify a range of volatile compounds such as alcohols, esters and hop derived aroma compounds. A simple and inexpensive conversion of a Gas Chromatography Flame Ionization Detector (GC FID) instrument to allow the use of Solid-Phase Microextraction was found to be useful for the quantification of volatile esters.

To study the spatial accessibility of healthcare services in cities on the Tibetan Plateau, this paper proposes an improved 3SFCA method in the main urban area of Xining City. The improved 3SFCA method incorporates both selection weights from the Huff model and the M2SFCA approach to addressing suboptimal allocation of supply resources. Results show that the accessibility of healthcare for the main urban area of Xining City decreases in a circle to four axes, with good accessibility in the east and center but poor accessibility in the north. And there is a positive spatial relationship between population and accessibility. Besides, this paper proposes a framework for studying the spatial accessibility of healthcare on the Tibetan Plateau.

Gangliosides are highly abundant in the human brain where they are involved in major biological events. In brain cancers, alterations of ganglioside pattern occur, some of which being correlated with the neoplastic transformation, while others with the tumor proliferation. Of all the techniques, mass spectrometry (MS) has proven to be one of the most effective in gangliosidomics, due to its ability to characterize heterogeneous mixtures and discover species with biomarker value. This review highlights the most significant achievements of MS in the analysis of gangliosides in human brain cancers. The first part presents the state-of-the-art in the MS development for discovery of ganglioside markers in primary brain tumors, with a particular emphasis on the ion mobility separation (IMS) MS and its contribution to the elucidation of the gangliosidome associated with aggressive tumors. The second part is focused on the MS of gangliosides in brain metastases, highlighting the ability of matrix-assisted laser desorption/ionization (MALDI)-MS, microfluidics-MS and tandem MS to decipher and structurally characterize species involved in the metastatic process. In the end, several conclusions and perspectives are presented, among which the need for development of a reliable software and a user-friendly structural database as a search platform in brain tumor diagnostics.

MALDI-TOF (Matrix-Assisted Laser Desorption/Ionization Time-of Flight) is a type of mass spectrometry (MS) that has been widely implemented for the rapid identification of microorganisms over the last decade. The accuracy and flexibility of this method has encouraged researchers to implement the analysis of protein spectra obtained by MALDI-TOF for the discrimination of close-related species and bacterial typing. In this study, a standardized methodology based on the detection of species-specific protein peaks from the spectra obtained with MALDI-TOF is described. The methodology was applied to a collection of Cryptococcus spp. (n=70) previously characterized by Amplified Fragment Length Polymorphism (AFLP) and sequencing of the ITS1-5.8S-ITS2 region. An expanded ad-hoc database was also built for their discrimination with MALDI-TOF. This approach did not allow the discrimination of the interspecies hybrids. However, the performance of peak analysis with the application of the PLS-DA and SVM algorithms in a two-step analysis allowed 96.95% and 96.55% correct discrimination of C. neoformans from the interspecies hybrids, respectively. Besides, PCA analysis prior to SVM provided 98.45% correct discrimination of the 3 analyzed species in a one-step analysis. The method is cost-efficient, rapid and user-friendly. The procedure can also be automatized for an optimized implementation in the laboratory routine.