TABLETS

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FORMULATIVE AND INDUSTRIAL PHARMACY,
FINAL BPHARM, NATIONAL COLLEGE OF PHARMACY
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FORMULATIVE AND INDUSTRIAL PHARMACY,
FINAL BPHARM, NATIONAL COLLEGE OF PHARMACY
 TABLETS

Tablets are solid, unit dosage forms containing one or more active ingredients along with suitable
excipientswhich are prepared by compression or by molding method.
Advantages:
1. They are unit dosage form with greatest precision and least content variability.
2. Their cost is lowest for all dosage forms. They are the lightest and most compact of all oral dosage
forms.
3. They are in general easiest and cheapest to pack and shipment of all oral dosage forms.
4. They tent themselves to certain special release profile product such as enteric or delayed release
product.
5. They are suitable for large scale production than other dosage forms.
Formulation:
Oral tablets usually contain the following components.
1. Diluents:They are fillers to make up the required bulk of the tablet when drug storage is inadequate
to produce their bulk.
Eg. Di basic calcium phosphate, Spray dried lactose.
2. Binders and adhesives:They are the materials added during the wet granulation method. To form
granule or to provide cohesive compact for directly compressed tablet.
Eg.Acacia, tragacanth, gelatin.
3. Disintegrants:They are added to facilitate the disintegration of the tablet when it contacts water in
GIT.Eg.Starch, modified starch.
4. Lubricants: They are the agents used to decrease the friction between the walls of the tablet and
the die cavity during tablet ejection.Eg. Modified starch, clays and bentonite.
5. Anti adhesives: These prevent the adhesion of the powder particles to the punch surface and die
cavity.Eg. Talc, Magnesium stearate
6. Glidents: These are agents which promote flow by decreasing the friction between individual
powder particles.Eg.Aerosil,carbosil
7. Colours,flavors and sweeteners:Colour should be approved by F.D & C.Flavouring oils are
used.Sweeteners are sucrose,mannitol.

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FORMULATIVE AND INDUSTRIAL PHARMACY,
FINAL BPHARM, NATIONAL COLLEGE OF PHARMACY
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FORMULATIVE AND INDUSTRIAL PHARMACY,
FINAL BPHARM, NATIONAL COLLEGE OF PHARMACY
Types of tablets

1. Tablet ingested orally

2. Tablet used in oral cavity

3. Tablet administered by other routes

4. Effervescent tablet

Granulation methods

1. Direct compression method

2. Wet granulation method

3. Dry granulation method

Evaluation Tests:
1) General appearance
 Size and shape
 Colour
 Identification of tablet
2) Hardness and friability
3) Weight variation
4) Disintegration
5) Dissolution

REFERENCE:

The theory and practice of industrial pharmacy by Leon Lachmann, 2009, Page no: 293-295.

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FORMULATIVE AND INDUSTRIAL PHARMACY,
FINAL BPHARM, NATIONAL COLLEGE OF PHARMACY
Observations and calculations

Specimen Label

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FORMULATIVE AND INDUSTRIAL PHARMACY,
FINAL BPHARM, NATIONAL COLLEGE OF PHARMACY
Experiment No: 1
Date:
PARACETAMOL TABLET I P (Wet granulation method)

Aim: To prepare and submit granules for 30 Paracetamol tablet each containing 500 mg of Paracetamol
and to carryout the evaluation test for granules.

Requirements: Paracetamol, acacia 2 %, mucilage of starch, magnesium stearate, purified talc, lactose.
Formula

Ingredients Official formula Working formula

Paracetamol

Diluents starch

Methyl paraben

Propyl paraben

Starch paste (10%)

Starch (disintegrant)

Talc

Magnesium Stearate

Principle: Paracetamol tablets are commonly used as analgesic and antipyretics. Starch powder acts as
a disintegrating agent. Starch paste is used as binding agent. Talc (1%) is used as glidant. Magnesium
stearate (1%) is added as lubricant.Paracetamol is not susceptible to moisture and temperature.
Therefore wet granulation method is suitable for granulation. Talc and magnesium stearate is added as
extragranular.

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FORMULATIVE AND INDUSTRIAL PHARMACY,
FINAL BPHARM, NATIONAL COLLEGE OF PHARMACY
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FORMULATIVE AND INDUSTRIAL PHARMACY,
FINAL BPHARM, NATIONAL COLLEGE OF PHARMACY
Procedure: Paracetamol tablets are prepared by wet granulation technique. Weighed out required
quantities of Paracetamol, diluent starch, methyl paraben and propyl paraben. Intimately mixthe
ingredients and passed it through sieve no: 44 to make it uniform size.Added starchpaste little by little
until coherent mass is obtained and pass through sieve number 10/12 and dry the granules at 600 C in
a hot air oven. The dried granules are taken out and pass it through sieve no 16 kept over sieve no 44.
The granules which are on sieve no 44 is taken as overs and powder below sieve no 44 is taken as
fines.15% of fines are added back to the overs and calculated the total final weight of granules. To this
granule, purified talc, starch (disintegrant) and magnesium stearate are added and mixed well.

The prepared granules are compressed using rotary tablet compression machine.

Evaluation of granules:

Determination of bulk density:

3tap method: Carefully introduce a sample of about 10g of granules, which has been previously
passed through a standard SieveNo. 20, into a 100ml graduated cylinder. Drop the cylinder onto a hard
wood surface 3 times from a height of 1inch at 2 second interval.The bulk density is then obtained by
dividing the weight of sample in grams by the final volume in cm3 of the sample contained in the
cylinder.

500tap method: Repeat the same procedure; here the cylinder has to be dropped or tapped
500times. It has been found that 500 tap method gives the most consistent results.

Determination of Compressibility Index:Gently pourapproximately 50ml of powder sample into

tarred graduated cylinder.Record the initial volume and the weight of powder.Determine the tapped
density(200)times same as in bulk density experiment.

Compressibility index =100 X Tapped density-Poured density

Tapped density

Hausner Ratio = Tapped density

Poured density

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FORMULATIVE AND INDUSTRIAL PHARMACY,
FINAL BPHARM, NATIONAL COLLEGE OF PHARMACY
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FORMULATIVE AND INDUSTRIAL PHARMACY,
FINAL BPHARM, NATIONAL COLLEGE OF PHARMACY
 Compressibility index(%) Flow character Hausner ratio

10 Excellent 1.00 - 1.11

11- 15 Good 1.12- 1.18

16-20 Fair 1.19- 1.25

21 -25 Passable 1.26- 1.34

26-31 Poor 1.35 -1.45

32- 37 Very poor 1.46 -1.59

˂ 38 Very very poor ˂ 1.60

Angle of repose: Fixa funnel at a particular height ‘h’cm on a burette stand. Placea white paper below
the funnel. Passthe given powdered drug whose angle of repose is to be determined, slowly through the
funnel until it forms a pile. Care is taken to see that the drug particles slip and roll over each other
through the side of the funnel. Further addition of drug is stopped as soon as the drug pile touches the
tip of the funnel.

Draw thecircumference of the pile of drug with a pencil without disturbing the pile. Note the radius of
the pile as ‘r’cm. Angle of repose θ0of this drug is then calculate by using the formula, θ=tan-1h/r

Dose: 0.5 – 1 gm
Storage: To be stored in a well closed light resistant container.
Use: Anti pyretic.
Report:

Reference: Pharmaceutics Practical manual by Dr. P Muthuprasanna, Page no; 38

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FORMULATIVE AND INDUSTRIAL PHARMACY,
FINAL BPHARM, NATIONAL COLLEGE OF PHARMACY
Observations and calculations

Specimen Label

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FORMULATIVE AND INDUSTRIAL PHARMACY,
FINAL BPHARM, NATIONAL COLLEGE OF PHARMACY
Experiment No: 2
Date:
SODIUM BICARBONATE TABLETS B.P

Aim:To prepare and submit granules for 30 sodium bicarbonate tablets BP each containing 300 mg of
sodium bicarbonate and to carryout the evaluation test for granules.

Synonyms: compound sodium bicarbonate tablets, soda mint tablets.

Formula as per B P
Ingredients Official formula
Sodium bicarbonate 0.300g
Starch paste q.s
Acacia 0.016 g
Sucrose 0.100 g
Menthol 0.001 g
Talc 2 % q.s
Peppermint oil 0.004 ml

Type: Heterogeneous powder – solid.

Requirements: Mortar and pestle, Beaker, measuring cylinder ,Watch glass, Sieves 10,22,44,60,
Compression machine, dryer.
Principle: Sodium bicarbonate tablets are used as antacids. These tablets are chewed. Chewing speeds
up disintegration and begins the wetting of drug. Hence there is no need of adding disintegrating agent.
Since the dose of sodium bicarbonate is high that is 300 mg, only small amount of additives particularly
diluents are required. The tablets should be palatable owing to chewing of the tablets. Sweetening
agents such as sucrose and mannitol provides pleasantness and also cooling sensation due to negative
heat of solution. Peppermint oil is used as the flavoring agent and also provides cooling effect to the
mouth. Menthol is used as a cooling agent, which enhances the effect of flavoring agent. The production
of chewable tablets involves wet granulation technique. This method is preferred, when the powders
have poor flow properties. The material to be compressed is expected to possess flowability and
compressibility in order to obtain good tablets.

Procedure : Calculate the working formula depending on the quantity of the tablets to be submitted.

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FORMULATIVE AND INDUSTRIAL PHARMACY,
FINAL BPHARM, NATIONAL COLLEGE OF PHARMACY
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FORMULATIVE AND INDUSTRIAL PHARMACY,
FINAL BPHARM, NATIONAL COLLEGE OF PHARMACY
Preparation of granulation medium (10 % starch paste): Weigh and transfer10 g of starch into a
beaker (250 ml). Add50 ml of water into the beaker and prepare the slurry by stirring with a glass rod.
Add25 ml of water into the beaker placed on a wire gauge. Heatthe slurry withBunsen burner to obtain
a thick paste. Add remaining 25 ml of water and stir well. Stop the heating andcool the starch paste.
Sifting of Powders: Mixthe sifted powders thoroughly with a mortar and pestle to obtain a uniform
blend.
Wet granulation: Takea small quantity of granulating medium into a watch glass and weigh. Transfer
little quantity of granulating medium to the mortar containing powders and triturate. Continue this
procedure until a smooth dough is formed. The end point to stop adding granulating medium is decided
by the following test.
Test Observation Inference
The wet mass is The ball crumbles under Stop adding granulating medium.
taken into hand and moderate pressure without giving The mass is ready for wet
a round ball is fines. screening.
made. It is pressed The ball breaks forming many Continue adding granulating
in the palm with the fines medium
thumb.

Pass the wet mass through 10 mesh sieve in a tray. This process breaks wet mass forming wet granules.
Wet granules surface area is more so that drying will be effective. Spreadthe wet granules in the tray.
Drying:Weigh the granulating medium left in the watch glass.Placethe tray containing granules in a
hot air oven and adjustthe temperature to 700C.
Dry screening:Weighthe total granules. Pass the dry granules through 22/44 mesh sieves completely.
Weigh the granules that are retained on 44 mesh sieve and these are coarse granules. Weigh the granules
that are passed through 44 mesh sieve. These are termed as fines. Calculate the percentage fines formed.
Dry blending:Calculate15% fines, weigh and add to the coarse granules. Add required quantities of
talc and flavoring agents.Blend the ingredients in order to get a uniform distribution of ingredients.
Now the granules are ready for compression.
Compression:Tablets with correct specifications are compressed using tablet compressing machine.

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FORMULATIVE AND INDUSTRIAL PHARMACY,
FINAL BPHARM, NATIONAL COLLEGE OF PHARMACY
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FORMULATIVE AND INDUSTRIAL PHARMACY,
FINAL BPHARM, NATIONAL COLLEGE OF PHARMACY
Evaluation of granules:
Determination of bulk density:
3tap method: Carefully introduce a sample of about 50cm3 of powder, which has been
previously passed through a standard SieveNo. 20, into a 100ml graduated cylinder. Drop the cylinder
onto a hard wood surface 3 times from a height of 1inch at 2 second interval.The bulk density is then
obtained by dividing the weight of sample in grams by the final volume in cm3 of the sample contained
in the cylinder.
500tap method: Repeat the same procedure; here the cylinder has to be dropped or tapped
500times. It has been found that 500 tap methods gives the most consistent results.

Determination of Compressibility Index:Gently pourapproximately 50ml of powder sample into

tarred graduated cylinder.Record the initial volume and the weight of powder.Determine the tapped
density(200)times same as in bulk density experiment.
Compressibility index =Tapped density-Poured density
Tapped density
Angle of repose: Fi xa funnel at a particular height ‘h’cm on a burette stand. Place a white paper below
the funnel. Passthe given powdered drug whose angle of repose is to be determined, slowly through the
funnel until it forms a pile. Care is taken to see that the drug particles slip and roll over each other
through the side of the funnel. Further addition of drug is stopped as soon as the drug pile touches the
tip of the funnel.

Draw thecircumference of the pile of drug with a pencil without disturbing the pile. Note the radius of
the pile as ‘r’cm. Angle of repose θ0of this drug is then calculate by using the formula, θ=tan-1h/r

Packing: compressed tablets are placed in wide mouthed container and the container is capped.

Labeling: Appropriate label is prepared and fixed to the container.

Composition:Each tablet contains 300 mg of sodium bicarbonate.

Category: Antacid and electrolyte replenisher.
Dose: 2 – 6 tablets a day

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FORMULATIVE AND INDUSTRIAL PHARMACY,
FINAL BPHARM, NATIONAL COLLEGE OF PHARMACY
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FORMULATIVE AND INDUSTRIAL PHARMACY,
FINAL BPHARM, NATIONAL COLLEGE OF PHARMACY
Storage:Preserve sodium bicarbonate tablets in a well closed container and in a cool place.

Auxiliary label:To be chewed in the mouth before swallow.

Date of expiry: 3 years from the date of manufacture

Report:

Reference: Laboratory Manual of Industrial Pharmacy, C V S Subrahmanyam, first edition, page no:

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FORMULATIVE AND INDUSTRIAL PHARMACY,
FINAL BPHARM, NATIONAL COLLEGE OF PHARMACY
Observations and calculations

Specimen Label

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FORMULATIVE AND INDUSTRIAL PHARMACY,
FINAL BPHARM, NATIONAL COLLEGE OF PHARMACY
Experiment No: 3
Date:
ASCORBIC ACID TABLETS I P
Aim:To prepare and evaluate 30 ascorbic acid tablets IP each containing 50 mg of ascorbic acid and
carry out the evaluation tests.
Synonyms:Vitamin C tablets,L-ascorbic acid tablets.
Formula as per I P
Ingredients Official formula

Ascorbic acid 50 mg
Lactose 250 mg
Methyl cellulose 5% q.s
PEG 4000,2% q.s
Note: To the above formula overages to the volume of 20 % are added to the quantity of ascorbic acid.
The working formula is calculated for 60 tablets.Extra 10 tablets are required to account for the
production losses.
Type: Heterogeneous powder – solid.
Requirements: Mortar and pestle, Beaker, measuring cylinder, Watch glass, Sieves 10,
22,44,60,Compression machine,dryer.
Principle: Ascorbic acid is used as Antiscorbotic and antioxidant. It is a water soluble vitamin.
Normally ascorbic acid oxidizes to dehydro ascorbic acid. Therefore care should be taken to prevent
oxidation of drug during manufacture. But during storage there is chance for the ascorbic acid to
undergo oxidation and therefore 20% overages are added to nullify loses during storage. Methyl
cellulose is used as granulating agent and vehicle should be non-aqueous base such as chloroform or
alcohol. When the dose of the active ingredient that is ascorbic acid is low large amount of water soluble
diluents is added. Diluents such as lactose can be included in the formulation. Since organic solvents
have low boiling points, drying of granules can be quick at a low temperature. Water soluble lubricants
such as PEG 4000 are used when soluble tablets are prepared.
Procedure: Calculatethe working formuladepending on the number of tablets to be submitted.
Preparation of granulation medium (5 % methyl cellulose):Weigh methyl cellulose powder (2.5g)
and transfer into a beaker (100 ml). Add little quantities of dry (water free) alcohol slowly with
continuous stirring. Finally, make up the volume (50 ml) to get desired concentration.

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FORMULATIVE AND INDUSTRIAL PHARMACY,
FINAL BPHARM, NATIONAL COLLEGE OF PHARMACY
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FORMULATIVE AND INDUSTRIAL PHARMACY,
FINAL BPHARM, NATIONAL COLLEGE OF PHARMACY
Sifting and blending of powders:Weigh the desired quantities of ascorbic acid and lactose as per the
working formula. Pass it through 60 mesh sieve. Mix the powders thoroughly in mortar in order to
obtain uniform mix of the material.

Wet granulation (wet screening):Take smallquantity of granulating medium into a watch glass and
weigh it. From thistransfer little quantity of granulating medium into the mortar containing powders
and triturate.Continuethe procedure until smooth dough is formed. The end point to stop adding
granulating medium is decided by the following test.
Test Observation Inference
The wet mass is taken The ball crumbles under Stop adding granulating medium.
into hand and a round moderate pressure without The mass is ready for wet
ball is made. It is pressed giving fines. screening.
in the palm with the
thumb. The ball breaks forming many Continue adding granulating
fines medium
Pass the wet mass through 10 mesh sieve in a tray. This process breaks wet mass forming wet granules.
Wet granules surface area is more so that drying will be effective. Spread wet granules in the tray.
Drying:Weigh the granulating medium left in the watch glass. Place the tray containing granules in a
hot air oven and dry at 40oC. Switch off the ovenand allow the granules to reach room temperature.
Dry screening:Weighthe total granules. Passthe dry granules through 22/44 mesh sieves completely.
Weigh the granules that are retained on 44 mesh sieve andthese are coarse granules.Weigh the granules
that are passed through 44 mesh sieve and these are termed as fines.Calculatethe percentage fines
formed.
Dry blending: Fifteen percentage fines are calculated weighed and added to the coarse granules. Add
required quantity of PEG 4000.Blend the ingredients in order to get a uniform distribution. Now the
granules are ready for compression.
Compression:Tablets with correct specifications are compressed using tablet compressing machine.
Evaluation:
Hardness test: Tablet hardness has been defined as the force required breaking a tablet in a diametric
direction. Hardness test can be conducted by either Pfizer hardness tester or Monsanto harness tester.
In both these instruments, place tablet between two anvils. ApplyForce toanvils andrecordthe crushing
strength that causes the tablet to break apart. Hardness is tablet crushing strength. Unit is Kg/cm2.

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FORMULATIVE AND INDUSTRIAL PHARMACY,
FINAL BPHARM, NATIONAL COLLEGE OF PHARMACY
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FORMULATIVE AND INDUSTRIAL PHARMACY,
FINAL BPHARM, NATIONAL COLLEGE OF PHARMACY
Friability test: Roche friabilator is used to measure the friability of tablets.It rotates at rate of
25rpm.Weighten tablets collectively and place in the chamber of friabilator. In the friabilator tablets
are exposed to rolling resulting from the free fall of tablets from a height of 6 inches within the chamber
of friabilator. After 100 rotations (4 minutes) take the tablets out from the friabilator and weigh the
tablets again. Friability can be determined using following formula. The weight lose should not be more
than 1%.
Friability = W1 –W2 ×100
W1
W1= Initial weight of the tablet.
W2= Final weight of the tablet.
Test for uniformity of weight (Weight variation test): Weigh twenty tablets individually.
Calculateaverage weight from the total weight of all tablets. Compareindividual weights with the
average weight. Percentage difference in weight variation should be within the prescribed limit. The
percentage deviation can be calculated using the following formula.
Percentage deviation = Individual weight – average weight x100
Average weight
The tolerance values of weight variation for uncoated tablet as per I P are as shown in the following
table.
Average Weight (mg) Percentage deviation
80 or less 10
More than 80 and less than 250 7.5
250 or more 5.0

The tolerance values of weight variation for uncoated tablet as per U S P are as shown in the following
table.
Average Weight (mg) Percentage deviation
Below 130 10
130 – 325 7.5
Above 325 5.0

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FORMULATIVE AND INDUSTRIAL PHARMACY,
FINAL BPHARM, NATIONAL COLLEGE OF PHARMACY
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FORMULATIVE AND INDUSTRIAL PHARMACY,
FINAL BPHARM, NATIONAL COLLEGE OF PHARMACY
Disintegration test: Disintegration test is determined using disintegration apparatus which consist of
a basket rack assembly containing 6 open ended glass tubes. They are held vertically and bottom of the
tube is covered with ten mesh sieves. Placeone tablet each in all six tubes.Place a disc to each tube over
the tablet and switch onthe apparatus. The tube travels upwards and downwards at a rate of 28-32
cycles/minute in water maintained at 37± 20C. Note the time taken for all the six tablets to break down
and pass through the mesh at the bottom of the tube. The tablets pass the test if all the six tablets
disintegrate within the prescribed time (15 minutes).If one or two tablets fail to disintegrate, the test is
repeated with another 12 tablets. The tablet passes the test if 16 out of 18 tablets disintegrate within
time.
Type Time of Disintegration
Uncoated tablets 15 minutes
Soluble tablets 3 minutes

Packing: Compressedtablets are placed in wide mouthed container and the container is capped.
Labeling:Appropriate label is prepared and fixedto the container.
Composition:Each tablet contains 50 mg of ascorbic acid.
Category: Anti scorbutic, anti-oxidant.
Dose:In the prevention of scurvy- 25 mg to 75 mg daily in divided doses.
In the treatment of scurvy-not less than 250mg daily in divided doses.
Storage:Store in a cool place.
Auxiliary label: To be chewed in the mouth or dissolve in water or keep the tablet in mouth to dissolve.
Date of expiry:1 years from the date of manufacture.
Report:

Reference: Laboratory manual of Industrial pharmacy by C V S Surahmanyam, first edition Page no;
16 – 19.

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FORMULATIVE AND INDUSTRIAL PHARMACY,
FINAL BPHARM, NATIONAL COLLEGE OF PHARMACY
Observations and calculations

Specimen Label

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FORMULATIVE AND INDUSTRIAL PHARMACY,
FINAL BPHARM, NATIONAL COLLEGE OF PHARMACY
Experiment No: 4

Date:
CALCIUM LACTATE TABLETS I P (Dry granulation method)
Aim: To prepare and submit 30 tablets of calcium lactate each containing 250 mg of calcium lactate IP
and carry out the evaluation tests.
Formula as per I P
Ingredients Official formula
Calcium lactate 0.300 g
Starch powder 0.015g
Talc 2% qs
Type: Heterogeneous powder – solid
Requirements: Mortar and pestle,Beaker, measuring cylinder, Watch glass, Sieves
10,22,44,60,Compression machine, dryer, calcium lactate, starch powder, talc.
Principle: Calcium lactate tablets are prepared using dry granulation or slugging method followed by
compression. Calcium lactate is hygroscopic. Wet granulation method is not suitable, because calcium
lactate becomes gummywhen water is added. Direct compression of material is not possible, because
it contains more number of fines and exhibit poor flow properties. Hence tablets of same hardness and
weight cannot be obtained.
In the dry granulation or slugging method, a blend of finely divided powders are forced into the dies of
larger capacity press and compacted by means of flat – faced punches with high pressure. These
compacted masses are called slugs. Slugs are hard and poorly formed tablets. These slugs are milled
and screened to get desired size granules. Talc is added to these granules and final compression is
attempted.
Procedure: Calculatethe working formuladepending on the number of tablets to be submitted.
Preparation of slugs: Weigh the desired quantities of calcium lactate and starch powder andpass
through 60 mesh sieve into a mortar.Trituratethe powdersin mortar to obtain uniform mix. Transfer the
mixed powders into hopper and compress with the help of bigger sized dies and punches.

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FORMULATIVE AND INDUSTRIAL PHARMACY,
FINAL BPHARM, NATIONAL COLLEGE OF PHARMACY
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FORMULATIVE AND INDUSTRIAL PHARMACY,
FINAL BPHARM, NATIONAL COLLEGE OF PHARMACY
Preparation of granules:Mill or powder the slugs in a mortar. Weighthe total granules. The granules
are passed through meshes 22/44. Granules that are retainedon 44 meshsieves are weighed and these
are coarse granules. The granules that are passed through 44 mesh sieve are weighed and these are
termed as fines. Percentage fines formed are calculated.

Dry blending:Fifteen percentage fines are calculated weighed and added to the coarse granules. Add
required quantity of talc.Blend the ingredients in order to get a uniform distribution. Now the granules
are ready for compression.
Compression: Three packets of granules, containing the practical weight of one tablet, are
prepared.These are used to adjust the pressure of the punches in order to get tablets of required hardness.
The remaining granules are compressed to obtain tablets.The practical yield is calculated.

Evaluation:
Hardness test: Tablet hardness has been defined as the force required to break a tablet in a diametric
direction. Hardness test can be conducted by either Pfizer hardness tester or Monsanto harness tester.
In both these instruments, place tablet between two anvils. ApplyForce toanvils andrecord the crushing
strength that causes the tablet to break apart. Hardness is tablet crushing strength. Unit is Kg/cm2.
Friability test: Roche friabilator is used to measure the friability of tablets.It rotates at rate of
25rpm.Weighten tablets collectively and place in the chamber of friabilator. In the friabilator tablets
are exposed to rolling resulting from the free fall of tablets from a height of 6 inches within the chamber
of friabilator. After 100 rotations (4 minutes) take the tablets out from the friabilator and weigh the
tablets again. Friability can be determined using following formula. The weight lose should not be more
than 1%.
Friability = W1 –W2 ×100
W1
W1= Initial weight of the tablet.
W2= Final weight of the tablet.

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FORMULATIVE AND INDUSTRIAL PHARMACY,
FINAL BPHARM, NATIONAL COLLEGE OF PHARMACY
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FORMULATIVE AND INDUSTRIAL PHARMACY,
FINAL BPHARM, NATIONAL COLLEGE OF PHARMACY
Test for uniformity of weight (Weight variation test): Weigh twenty tablets individually.
Calculateaverage weight from the total weight of all tablets. Compareindividual weights with the
average weight. Percentage difference in weight variation should be within the prescribed limit. The
percentage deviation can be calculated using the following formula.

Percentage deviation = Individual weight – average weight

Average weight
The tolerance values of weight variation for uncoated tablet as per I P are as shown in the
followingtable.

Average Weight (mg) Percentage deviation

80 or less 10
More than 80 and less than 250 7.5
250 or more 5.0
The tolerance values of weight variation for uncoated tablet as per U S P are as shown in the following
table.
Average Weight (mg) Percentage deviation
Below 130 10
130 – 325 7.5
Above 325 5.0

Disintegration test: Disintegration test is determined using disintegration apparatus which consist of
a basket rack assembly containing 6 open ended glass tubes. They are held vertically and bottom of the
tube is covered with ten mesh sieves. Placeone tablet each in all six tubes.Place a disc to each tube over
the tablet and switch onthe apparatus. The tube travels upwards and downwards at a rate of 28-32
cycles/minute in water maintained at 37±0.50C. Note the time taken for all the six tablets to break down
and pass through the mesh at the bottom of the tube. The tablets pass the test if all the six tablets
disintegrate within the prescribed time (15 minutes).If one or two tablets fail to disintegrate, the test is
repeated with another 12 tablets. The tablet passes the test if 16 out of 18 tablets disintegrate within
time.
Type Time of Disintegration
Uncoated tablets 15 minutes
Soluble tablets 3 minutes

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FORMULATIVE AND INDUSTRIAL PHARMACY,
FINAL BPHARM, NATIONAL COLLEGE OF PHARMACY
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FORMULATIVE AND INDUSTRIAL PHARMACY,
FINAL BPHARM, NATIONAL COLLEGE OF PHARMACY
Packing: Compressed tablets are placed in wide mouthed light resistant container and the container is
capped.
Labeling:Appropriate label is prepared and fixed to the container.
Composition: Each tablet contains 300 mg of calcium lactate penta hydrate.
Category: Calcium replenisher.
Dose: Up to 8 g daily in divided doses.
Storage: Store in a tightly closed container.
Auxiliary label: Tobe chewed in the mouth before swallow.
Date of expiry: 18 months from the date of manufacture

Report:

Reference:Laboratory Manual of Industrial Pharmacy by C V S Subrahmanyam, first edition, Page no;

21-24.

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FORMULATIVE AND INDUSTRIAL PHARMACY,
FINAL BPHARM, NATIONAL COLLEGE OF PHARMACY
Observations and calculations

Specimen Label

36
FORMULATIVE AND INDUSTRIAL PHARMACY,
FINAL BPHARM, NATIONAL COLLEGE OF PHARMACY
Experiment No: 5
Date:
FERROUS SULPHATE TABLETS (wet granulationmethod)
Aim: To prepare and submit granules for 30 ferrous sulphate tablets each containing 300 mg of ferrous
sulphate carry out the evaluation test for granules.
Formula as per I P
Ingredients Official formula
Ferrous sulphate 300 mg
Sugar solution q.s 10%
Starch 9 mg
Magnesium stearate q.s 1%
Talc q.s 2%
Principle:Ferrous sulphate tablets are prepared by wet granulation method. In this sugar solution is
used as granulating agent.It should be prepared before the process.The wet granulation process is
completed in 5 steps weighing,mixing,granulating,compressing and ejecting.In this preparation, starch
solution is used as binding agent and granulating agent.Addition of improper amount of granulating
agent leads to capping and lamination.Talc is used as glidant to improve flow property.Magnesium
sulphate is used as lubricant and it helps in tablet ejection from cavity.Lubricant decreases the friction
between dyes and punches.Proper drying is essential because improper drying leads to picking and
sticking.Over drying leads to breaking.
Procedure:Mix ferrous sulphate and starch with sugar solution and then pass through sieve number
10.Pass thegranules through sieve number 22 and 44 respectively to separate coarse and fines.Calculate
15 % fines and add into coarse granules. Calculatethe practical weight.Add talc and magnesium stearate
and then compress into tablets.
Evaluation of granules:
Determination of bulk density:
3tap method: Carefully introduce a sample of about 50cm3 of powder, which has been
previously passed through a standard SieveNo. 20, into a 100ml graduated cylinder. Drop the cylinder
onto a hard wood surface 3 times from a height of 1inch at 2 second interval.The bulk density is then
obtained by dividing the weight of sample in grams by the final volume in cm3 of the sample contained
in the cylinder.

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 500tap method: Repeat the same procedure; here the cylinder has to be dropped or tapped
500times. It has been found that 500 tap method gives the most consistent results.

Determination of Compressibility Index:Gently pourapproximately 50ml of powder sample into

tarred graduated cylinder.Record the initial volume and the weight of powder.Determine the tapped
density(200)times same as in bulk density experiment.

Compressibility index =Tapped density-Poured density

Tapped density

Angle of repose: Fixa funnel at a particular height ‘h’cm on a burette stand. Place a white paper below
the funnel. Passthe given powdered drug whose angle of repose is to be determined, slowly through the
funnel until it forms a pile. Care is taken to see that the drug particles slip and roll over each other
through the side of the funnel. Further addition of drug is stopped as soon as the drug pile touches the
tip of the funnel.

Draw thecircumference of the pile of drug with a pencil without disturbing the pile. Note the radius of
the pile as ‘r’cm. Angle of repose θ0of this drug is then calculate by using the formula, θ=tan-1h/r
Category: In the treatment of iron deficiency anemia.
Dose:Two tablets daily.
Storage: To be stored in a cool place.
Report:

Reference: Pharmaceutics practical manual by Dr.PMuthuprasanna, Page no; 41

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Observations and calculations

Specimen Label

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Experiment No: 6
Date:
ASPIRIN TABLET

Aim: To prepare and submit 30 tablets of aspirin each containing 300 mg of Aspirin and carry out the
evaluation tests for tablets.
Principle: Aspirin can be directly compressed without going for the granulation process. In the direct
compression, the process includes weighing mixing and compression only glidents and lubricants area
added depending up on the requirements. Aspirin capsules are used for its analgesic and antipyretic
activity. Direct compression method is an economic and quick method of production because number
of steps involved is less s compared to dry and wet granulation method. Since the dose of aspirin is
300mg only small amount of additives such as microcrystalline cellulose and spray dried lactose are
used .Starch is used as disintegrating agent. Talc is used as lubricant.

Procedure: Depending up on the number of tablet to be submitted the working formula is calculated.
Weighing: Granular acetyl salicylic acid is weighed approximately.
Screening: Weighed aspirin is passed to 22/44 mesh sieve. The material retained on the 44 mesh is
collected and is called as coarse granules and 15% fine required are weighed. 5 % of starch powder and
2 % of talc powder are weighted.
Blending:Coarse and fine granules, starch powder, talc powder are blended thoroughly in a mortar and
pestle to get uniform distribution of ingredients. Now granules are ready for compression.

Compression:Three packets of granules each containing the practical weight of one tablet is
prepared.They are used to adjust the pressure of the punches in order to get tablet of sufficient hardness.
The remaining granules are compressed to obtain granules.
Evaluation:
Test for uniformity of weight (Weight variation test): Weigh twenty tablets individually.
Calculateaverage weight from the total weight of all tablets. Compareindividual weights with the
average weight. Percentage difference in weight variation should be within the prescribed limit. The
percentage deviation can be calculated using the following formula.

Percentage deviation = Individual weight – average weight

Average weight

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The tolerance values of weight variation for uncoated tablet as per I P are as shown in the following
table.
Average Weight (mg) Percentage deviation
80 or less 10
More than 80 and less than 250 7.5
250 or more 5.0
The tolerance values of weight variation for uncoated tablet as per U S P are as shown in the following
table.
Average Weight (mg) Percentage deviation
Below 130 10
130 – 325 7.5
Above 325 5.0
Hardness test: Tablet hardness has been defined as the force required to break a tablet in a diametric
direction. Hardness test can be conducted by either Pfizer hardness tester or Monsanto harness tester.
In both these instruments, place tablet between two anvils. ApplyForce toanvils andrecord the crushing
strength that causes the tablet to break apart. Hardness is tablet crushing strength. Unit is Kg/cm2.
Friability test: Roche friabilator is used to measure the friability of tablets.It rotates at rate of
25rpm.Weighten tablets collectively and place in the chamber of friabilator. In the friabilator tablets
are exposed to rolling resulting from the free fall of tablets from a height of 6 inches within the chamber
of friabilator. After 100 rotations (4 minutes) take the tablets out from the friabilator and weigh the
tablets again. Friability can determine using following formula. The weight lose should not be more
than 1%.
Friability = W1 –W2 ×100
W1
W1= Initial weight of the tablet.
W2= Final weight of the tablet.

Disintegration test: Disintegration test is determined using disintegration apparatus which consist of
a basket rack assembly containing 6 open ended glass tubes. They are held vertically and bottom of the
tube is covered with ten mesh sieves. Placeone tablet each in all six tubes.Place a disc to each tube over
the tablet and switch onthe apparatus. The tube travels upwards and downwards at a rate of 28-32
cycles/minute in water maintained at 37±0.50C. Note the time taken for all the six tablets to break down
and pass through the mesh at the bottom of the tube. The tablets pass the test if all the six tablets
disintegrate within the prescribed time (15 minutes).If one or two tablets fail to disintegrate, the test is
repeated with another 12 tablets. The tablet passes the test if 16 out of 18 tablets disintegrate within
time.

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 Type Time of Disintegration
Uncoated tablets 15 minutes
Soluble tablets 3 minutes

Packing:The compressed granules are placed in wide mouthed tightly closed container it capped and
cleaned.

Category:Analgesic,Antipyretic,Anti Thrombotic

Storage:Stored in tightly closed container

Report:

Reference:Lab manual of industrial pharmacy by C.V.S.Subramanium, 1st edition, page no

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Observation and calculation

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Experiment No: 7
Date:
TEST FOR UNIFORMITY OF WEIGHT (Weight variation test)

Aim: To find out the weight variation of tablets in a given batch.

Principle:Any variation in the tablet weight leads to over dose or under medication.Weight variation
test is an in process quality control test controlled when tableting is under process.This test should be
conducted quickly without wasting time, can be carried out in every hour during the tablet
manufacturing process. Corrections are made during the compression of the tablet. Variation in weight
of tablet by any reason may lead to overdose. According to IP if weight is less than 80mg 10 percent
variation,if weight is between 80-250mg the percentage allowed is 7.5 %.If weight is more than 250mg
5% variation is allowed. Improper flow of granules from the hopper is responsible for the weight
variation. Lubricants, glidents and optimum amount of fines help to increase flow properties.
Procedure:Weigh twenty tablets individually. Calculate average weight from the total weight of all
tablets. Compare individual weights with the average weight. Percentage difference in weight variation
should be within the prescribed limit. The percentage deviation can be calculated using the following
formula.
Percentage deviation = Individual weight – average weight
Average weight
The tolerance values of weight variation for uncoated tablet as per I P are as shown in the following
table.
Average Weight (mg) Percentage deviation
80 or less 10
More than 80 and less than 250 7.5
250 or more 5.0
The tolerance values of weight variation for uncoated tablet as per U S P are as shown in the following
table.
Average Weight (mg) Percentage deviation
Below 130 10
130 – 325 7.5
Above 325 5.0
Report:

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Observation and calculation

Sample no: Hardness

10

Average Hardness

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Experiment No: 8
Date:
HARDNESS TEST

Aim: To find out the hardness of the prepared tablet.

Principle: Hardness is a force required to break a tablet across the diameter. The hardness of a tablet
is an indication of its strength. The tablet should be stable to mechanical stress during handling and
transportation. The degree of hardness varies with the different manufacturers and with the different
types of tablets. The force is measured in kilograms and the hardness of about 4 kg is considered to be
satisfactory for uncoated tablet. It is tested using hardness testers such as Monsanto tester Pfizer tester,
Erweka tester, Schleuniger tester and strong cob tester. Depending upon the type and concentration of
the binding agent used the hardness of the tablet varies.

Procedure: Tablet hardness has been defined as the force required to break a tablet in a diametric
direction. Hardness test can be conducted by either Pfizer hardness tester or Monsanto hardness tester.
In both these instruments,place tablet between two anvils.Apply force to anvils and crushing strength
that causes the tablet to break apart is recorded. Hardness is tablet crushing strength. Unit is Kg/cm2.

Report:

Reference: Pharmaceutics practical manual by Dr. PMuthuprasanna, Page no; 43

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Observation and calculation

Initial Final Friability %

(w1) - (w2)
weight weight (w1) - (w2) (w1) - (w2) x100
(w1)
(w1) (w2) (w1)

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Experiment No: 9
Date:
FRIABILITY TEST

Aim: To find out the percentage of friability in the given batch of tablets.

Principle:Friability is the loss of weight of tablet in the container du to removal of fine particle from
the surface. Roche friabilator is used to measure the friability of tablets .It is to ensure the ability of the
tablet to withstand the shocks during processing.

Procedure:Roche friabilator rotates at rate of 25 rpm.Weighten tablets collectively and place in the
chamber of friabilator. In the friabilator tablets are exposed to rolling resulting from the free fall of
tablets from a height of 6 inches within the chamber of friabilator. After 100 rotations (4 minutes) take
the tablets out from the friabilator and weighagaintablets collectively. Friability can be determined
using following formula. The weight lose should not be more than 1%.

Friability = W1 –W2 ×100

W1

W1= Initial weight of the tablet.

W2= Final weight of the tablet.

Report:

Reference: Pharmaceutics practical manual by Dr. PMuthuprasanna, Page no; 44

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Observation and calculation

Sample no: Disintegration time

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Experiment No: 10
Date:
DISINTEGRATION TEST
Aim: To carry out the disintegration test for the given uncoated tablets.
Principle:Disintegration test is determined using disintegration apparatus which consist of a basket
rack assembly containing 6 open ended glass tubes. They are held vertically and bottom of the tube is
covered with ten mesh sieves. One tablet each is placed in all six tubs. A disc to each tube is placed
over the tablet and the apparatus is switched on. The tube travels upwards and downwards at a rate of
28-32 cycles/minute in water maintained at 37±0.50C. The time taken for all the six tablets to break
down and pass through the mesh at the bottom of the tube is noted. The tablets pass the test if all the
six tablets disintegrate within the prescribed time (15 minutes).If one or two tablets fail to disintegrate,
the test is repeated with another 12 tablets. The tablet passes the test if 16 out of 18 tablets disintegrate
within time.

Procedure: Disintegration test is determined using disintegration apparatus which consist of a basket
rack assembly containing 6 open ended glass tubes. They are held vertically and bottom of the tube is
covered with ten mesh sieves. Placeone tablet each in all six tubs. A disc to each tube is placed over
the tablet and the apparatus is switched on. The tube travels upwards and downwards at a rate of 28-32
cycles/minute in water maintained at 37±0.50C. The time taken for all the six tablets to break down and
pass through the mesh and the bottom of the tube is noted. The tablets pass the test if all the six tablets
disintegrate within the prescribed time (15 minutes).If one or two tablets fail to disintegrate, the test is
repeated with another 12 tablets. The tablet passes the test if 16 out of 18 tablets disintegrate within
time.

Type Time of Disintegration

Uncoated tablets 15 minutes
Soluble tablets 3 minutes
Report:

Reference: Pharmaceutics practical manual by Dr. P Muthuprasanna, Page no; 44

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Observation and calculation

Standard graph

Concentration
Absorbance
(µg/ml)

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Experiment No: 11
Date:
DISSOLUTION TEST

Aim: To carry out the dissolution test of paracetamol tablets.

Principle:Dissolution rate may be defined as the amount of drugthatgoes into solution per unit time
under standardized conditions ofliquid or solid interface, temperature and solvent composition.
Noyes Whitney’s equation is useful for estimating the rate of reaction.(dC/dt)
dC/dt= KS(Cs-C) C -Con of drug dissolved
S - Surface area of particles
Cs -Equilibrium solubility
t -time
K –Proportionality constant
In the above equation, the concentration gradient is a variable and other terms are constant. Noyes
Whitney’s equation describes first order dissolution kinetics. When the concentration is plotted against
time a curvilinear plot will be obtained.
Tablet dissolution is the standard method for measuring the rate of drug release from a dosage form.
The dissolution rate predicts the rate and extent of drug absorption.

Importance: - It is an indirect measure of bioavailability.

-To ensure 100% release of drug from the dosage form.
- To ensure batch to batch uniformity in release.
Acceptance table
Number
Stage Acceptance criteria
tested
S1 6 Each unit is not less than D* + 5%
S2 6 Average of 12 units (S1+S2) is equal to or greater than D, and no unit is less
than D-15 %
S3 12 Average of 24 units (S1+S2 +S3) is equal to or greater than D , Not more than
2 units are less than D-15 % and not unit is less than D-25 %
D* is the amount of dissolved active ingredient specified in the individual monograph, expressed as a
percentage of the stated amount.

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Procedure:
Preparation of standard curve:Accurately weigh100mgo fParacetamol pure powder, add50ml of
0.1N sodium hydroxide solution to it and make up to 100ml with distilled water. This is considered as
stock solution. From this stock solution 1ml was taken and diluted to 100ml. Then from this solution
pipetteout2, 4, 6, 8 & 10ml and make up to 10ml with distilled water so as to obtain 2, 4, 6, 8, and 10
µg/ml andmeasure the absorbance at 243nm. From the standard graph slope value can be calculated.

Dissolution study:

1) Take Paracetamol tablets and place one in each basket of the dissolution assembly filled with
phosphate buffer pH 5.8 maintained at 37oC and using paddle rotated at 50 rpm.
2) Collectabout 2.0 ml samples at definite intervals and filterthe samples anddilute 1.0 ml sample to
100 ml with drug free buffer and then measure absorbance at 243.0 nm and calculatethe cumulative
percentage release.

Report:

Reference: Indian Pharmacopoeia 1996 volume II, Page no: 556.

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Observations and calculations

Specimen Label

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Experiment No: 12
Date:
ASPIRIN CAPSULES U S P

Aim:To prepare and submit 100 capsules USP each containing 300 mg of aspirin.
Synonym: Acetyl salicylic acid capsules.
Formula as per I P

Ingredients Official formula Working formula

Acetyl salicylic acid 0.3 g
Starch 0.03 g

The working formula is calculated for 110 capsules. Extra 10 capsules are required to account for the
production losses.
Principle: Aspirin is used as an analgesic in the dose of 0.3 g. It is slightly bitter in taste. Hence 0.3 g
of aspirin capsules can be placed in hard gelatin capsules which also serve to mask the bitter taste.
Capsules have been reported to produce both poorer and better absorption rates than tablets of a
particular drug. Size 1 capsules capacity for aspirin is 0.33 g. As the dose is 0.3 g, the diluents starch
is used to increase the weight of the capsules can be manufactured by manual technique using hand
operated capsule filling machine. Capsules are unsuitable for the administration of very soluble
compounds such as potassium chloride, calcium chloride, potassium bromide and ammonium bromide.
In such cases when the partly dissolved contents of capsule come in contact with the stomach wall, the
concentrated solution may cause localized irritation and gastric distress.

Type: Heterogeneous powder – Solid

Apparatus and chemicals: Hand operated capsule filling machine.Emptygelatine capsules, aspirin
powder and starch powder.
Procedure: Selectempty capsules of required size. Fill the capsules into the loading trays of the filling
machine. The cam handle is operated to hold the bodies of the capsules.Liftthe loading tray to separate
caps from bodies. Place the powder tray in position and spreadthe aspirin powder uniformly. Scrap the
excess powder towards platform of the powder tray. The pin plate is brought into position to press the
powder uniformly. Raise the pin plate and fill the remaining powder into the bodies of capsules. Repeat
this step until the powder is completely filled. Remove the powder tray.Place the cap holding tray

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into the position. Then the plate with rubber top is lowered and the liver is locked to join the cap and
bodies firmly.
The liver is unlocked and the plate with rubber top is lifted.The discharge handle is operated to push
the filled capsules out. The capsules are collected. The filled capsules are subjected to dusting in
cloth. The capsules are polished by rubbing them with gloves containing muslin cloth. The capsules
are placed in wide mouthed air tight container labeled and submitted.

Composition:Each capsule contains 0.3 g of aspirin.

Category:Analgesic, anti-pyretic, anti-rheumatic, and anti-thrombolytic.

Dose: As analgesic and anti-pyretic: 0.3 g – 0.6 g four to six times a day.

As anti-rheumatic, 1-2 g four to six times a day up to 10 g daily.

Storage: Stored in a well closed container in a cool and dry place.

Auxiliary label: Not to be used in children below 12 years of age except under medical advice.

Dateof expiry: 12 months from the date of manufacture.

Report:

Reference: Laboratory manual of industrial pharmacy by C V S Subrahmanyam, Page no: 57-60.

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 INJECTIONS

Injections or parenteral preparations are those preparations which are injected in to the blood with the
help of a needle. They are injected under through one or more layers of the skin. They should be sterile
therefore called as sterile products.

Classification

Based on the volume of the preparation that is placed in the container,they are classified as

1. Small volume parenterals(SVP)

2. Large volume parenterals (LVP)

Quality control test:

They should be free from all type of living organisms. They should be isotonic with the body fluids.
They are evaluated as

1. Pyrogen test
2. Sterility test
3. Clarity test
4. Leaker test

Reference:Lab manual for Industrial pharmacy by C.V.S.Subramaniyam, Page no.74-76.

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Observations and calculations

Specimen Label

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Experiment No: 13
Date:
ASCORBIC ACID INJECTION I P
Aim: To prepare and submit 2 ampoules each containing 2 ml of ascorbic acid injection I P.
Formula as per I P
Ingredients Official formula Overages
Ascorbic acid 25.00 g 3.75 g
Sodium bicarbonate 14.58 g
P-chlorometa cresol 0.1 g
Water for injection q.s to 100 ml

Type: Monophasic liquid dosage form – solution.

Principle: Ascorbic acid is a strong anti oxidant (reducing agent). Both ascorbic acid and de-hydro
ascorbic acid are biologically active. Sterilization by autoclaving is not possible owing to its
decomposition. Hence aseptic filling and filtration are available. To prevent the decomposition of
ascorbic acid during steaming a preservative is added. Ascorbic acid gradually darkens on exposure to
light. Intramuscular injection of ascorbic acid is preferred, but it may also be given subcutaneously or
intravenously. Intravenously, it can be added to a large volume of compatible diluents and infused
slowly.
Procedure:Depending on the number of injections to be submitted, the working formula is calculated.
The manufacturing operations are done in clean rooms.
Cleaning of ampoules: Clean three ampoules of type I glass thoroughly with detergent solution, then
with tap water and finally with distilled water. Keep the ampoules in an inverted position in a beaker
containing distilled water.Boilthe water for 15 minutes,removethe ampoules and dry in a hot air oven.
Preparation of ascorbic acid solution
1. Place 2/3rd of the total volume of water in a beaker.
2. Weighascorbic acid and suspend in water with continuous stirring.
3. Slowly addsodium bicarbonate with vigorous stirring. Effervescence is produced
4. After subsiding the effervescence, addremaining NaHCO3. Continuethis process till ascorbic acid
completely dissolves.
5. Add Para chlorometacresol andstir to dissolve.
6. Adjust the pH to 5.7 and filter the solution through G-4 filter.

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Filling into ampoules: Rinse the syringe with water for injection followed by rinsing with drug
solution. Loadthe syringe with the drug solution.Remove theair bubbles. This can be achieved by
tapping the syringe with finger, while holding it in perfectly vertical position. After expelling the air at
least one drop of drug solution should be expelled. After this adjustment the volume indicates the
desired quantity of liquid in ml. Then transferthe drug solution into the ampoules slowly by inserting
the needle up to the bottom of the container. Therefore a needle larger than the length of ampoule is
necessary. This prevents the rim (or neck) from contaminating by drug solution and also prevents the
charring of solution.

Sealing of ampoules:The ampoules can be sealed by using pull sealing technique.

Sterilization:The sealed ampoules are sterilized by steaming for 30 minutes.

Packing:Ampoules are packed in a suitable ampoule box and labeled

Composition:Each ml contains 250 mg of ascorbic acid.

Category:Antiscorbutic (ascorbic acid is used in the treatment and prevention of scurvy).

Doses: Prophylactic dose 25 – 75 mg daily.

Therapeutic dose – Not less than 250 mg daily in divided doses

Storage: Store in a cool and dark place not exceedingtemperature of 700C.

Auxiliary label:Discard if any particulate matter is present.

Precaution:Since pressure may develop on long storage, precautionshould be taken to wrap the
container in a protective covering while it is being opened.

Route of administration: Intramuscular route.

Date of expiry: 3 years from the date of manufacture.

Report:

Reference:Laboratory manual of Industrial pharmacy by C V S Surahmanyam,First edition

Page no: 78–84.

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Observations and calculations

Specimen Label

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Experiment No: 14
Date:
CALCIUM GLUCONATE INJECTION I P
Aim: Toprepare and submit 2 ampoules each containing 10 ml of calcium gluconate I P.
Formula as per I P
Ingredients Official formula
Calcium gluconate 9.65 g
Calcium D - Saccharate 0.35 g
Water for injection q.s 100 ml

Type: Monophasic liquid dosage form.

Principle: Calcium gluconateis slowly soluble in about 30 parts of water and soluble in 5 parts of
boiling water. Calcium in the form of calcium gluconate is used in the strength of 10 % w/v. In fact
10% solution of calcium gluconate in water gives a saturated solution. Any temperature fluctuation
during storage results in the crystallization of calcium gluconate. Therefore IP prescribes to replace a
part of calcium gluconatelactobionate (not more than 5 % of the total) by an equal amount of more
soluble calcium salt, such as calcium D Saccharate or calcium lactobionate. These soluble calcium salts
are known as stabilizing agents. Calcium gluconate is usually administered intravenously as a 10%
solution, slowly by direct intravenous injection, or by continuous or intermittent intravenous injection.
Calcium gluconate is incompatible with substances such as metaclopramideHCl, Indomethacin sodium
trihydrate, citrates soluble carbonates phosphates and sulphates.

Procedure:Calculate the working formula depending on the number of injections to be submitted. The
manufacturing operations are done in clean rooms.
Cleaning of ampoules: Cleaning of type I glass ampoule is carried out by following the usual
procedure.
Preparation of calcium gluconate injection
1. Accurately weighthe desired amount of calcium gluconate and calcium D–saccharate.
2. On account of the solubility problems, first dissolvecalcium gluconate in water for injection in
beaker with aid of heat.
3. Then dissolvecalcium D–saccharatein the above solution.
4. Coolthe solution.

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 5. After cooling, filterthe drug solution through G-4 filter to remove any foreign particles.

Filling into ampoules:Filling of ampoules is done following the usual procedure.

Sealing of ampoules the ampoules:The ampoules can be sealed by using pull sealing technique.

Sterilization:In general calcium gluconate injection is subjected to terminal sterilization. This can be
achieved by autoclaving at 121 0C at 15 lbs/ inch 2for 30 minutes.

Report:

Reference:Laboratory manual of Industrial pharmacy by C.V.S Subrahmanyam, First edition, Page

no:85-88.

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Observations and calculations

Specimen Label

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Experiment No: 15
Date:
ATROPINE SULPHATE INJECTION I P
Aim: To prepare and submit 2 ampoules each containing 2 ml of atropine sulphate injection I P
Formula as per I P
Ingredients Official formula
Atropine sulphate 0.05 g
Water for injection q s 100 ml
Type:Monophasic liquid dosage form – solution.
Principle: Atropine is an alkaloid which is normally insoluble in water. Therefore a salt of atropine,
i.e atropine sulphate is preferred owing to its greater aqueous solubility. It is soluble in 0.5 parts of
water. Atropine undergoes hydrolysis to yield tropane and tropic acid. Therefore during autoclaving
care should be taken to strictly adhere to the sterilization conditions. The pKa of atropine is 9.65.
Atropine sulphate in aqueous solution gives acidic pH and it varies from 4.0 to 6.0.

Procedure: Calculate the working formula depending on the number of injections to be submitted. The
manufacturing operations are done in clean rooms.
Cleaning of ampoules:Clean three ampoules of type I glass thoroughly with detergent solution, then
with tap water and finally with distilled water. Keep the ampoules in an inverted position in a beaker
containing distilled water.Boilthe water for 15 minutes, removethe ampoules and dry in a hot air oven.
Preparation of atropine sulphate solution:Accurately weigh the desired amount of atropine sulphate.
Dissolvethis in the desired amount of water for injection. Filter the solution using G-4 filter (or
Whatmann filter paper) to remove any foreign particles.

Filling into ampoules: Rinsethe syringe with water for injection followed by rinsing with drug
solution. Loadthe syringe with atropine sulphate solution and transfer into the ampoules slowly by
inserting the needle up to the bottom of the container.

Sealing of ampoules: The ampoules can be sealed by using pull sealing or tip sealing technique.

Sterilization:Atropinesulphateinjection is subjected to terminal sterilization. This can be achieved by

autoclaving at 121 0C at 15 lbs/inch2for 30 minutes. Filtration method can also be used.

Packing:Ampoules are packed in a suitable ampoule box (light resistant) and labeled.

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Composition: Each ml contains 0 5 mg of atropine sulphate.

Category: Anticholinergic, antidote to cholinesterase inhibitors.

Doses: 0.4–0.6 mg four to six times a day as anti-dote to cholinesterase inhibitors by intravenous
injection,2–4 mg initially followed by intramuscular injection,2 mg repeated for every 5–10 minutes.

Storage: Store in a cool place.

Auxiliary label: Discard if any particulate matter is present.

Route of administration: SC, IM or IV.

Date of expiry: 3 years from the date of manufacture.

Report:

Reference:Laboratory manual of Industrial pharmacy by C V S Subrahmanyam, first edition, Page no:

93-95.

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Observation and calculation

Ampoule Particulate matter

Inference
no: White background Black background

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Experiment No: 16
Date:
CLARITY TEST

Aim:To evaluate presence of particulate matter in parenteral product.

Principle:It is done to evaluate the presence of particulate matter in the parentral products.The visual
inspection of product container is usually done by individual human inspection of each externally
closed container under a good baffled against reflection in to the eye and viewed against a white and
black background with eye and content set in motion with a swirling action. A moving particle is much
easier to see than the stationary particle. It utilizes the principle of light scattering.

Procedure: Ampoules containing formulations can be tested by visual examination with the aid of
direct lighting; the product is placed against black and white backgrounds. Transparent particles are
visible in black background and opaque particles are visible in white background.

Report:

Reference:The theory and practical of industrial pharmacy by Leon Lachman, Page no: 673.

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Observation and calculation

Ampoule no: Observation Inference

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Experiment No: 17
Date:
LEAKER TEST FOR CONTAINERS

Aim:To perform leaker test for the given ampoules.

Requirements: Ampoules, distilled water, methylene blue, beaker, autoclave.

Principle: Ampoules are intended to provide a hermetically sealed container for a single dose product,
thereby completely barring any interchange between the contents of sealed ampoule and environment.
Changes in temperature show expansion and contraction of ampoules. Capillary pores or tiny cracks
may present through which microorganisms or other dangerous contaminants may enter the ampoules.
The leaker test is intended to detect incompletely sealed ampoules so that they may be discarded. Tip
sealed ampoules are more likely to be incompletely sealed than those that have been pull sealed. In
addition, small cracks may occur around the seal or at the base of ampoule as a result of improper
handling.

Leaks are detected by producing a negative pressure within incompletely sealed ampoules,
while ampoule is entirely submerged in a deeply coloured dye solution (0.5%-1% methylene
blue).Subsequent atmospheric pressure causes the dye to penetrate an opening, being visible after
ampoule has been washed externally to clear it off dye. Only a tiny drop of dye may penetrate a small
opening.

Advantages
 Both leaker detection and sterilization can be done in one operation.
Disadvantages
 Capillaries of about 15 µ in diameter or smaller may or may not be detected by these methods.
 Vials and bottles not subjected to such a leaker test because rubber closures are not rigid.

Procedure: Rinse the ampoules twice with distilled water. Then fill the ampoules to the brim with the
distilled water, empty them and determine the average overflow volume. Again fill the ampoules with
the average overflow volume of distilled water and seal them by fusion method.Entirely submerge
theampoules in a deeply coloured dye solution.(0.5%-1% - methylene blue) taken in a beaker. Place it
in autoclave. Close the autoclave and displace the air by passage of steam for 10minutes, raise the
temperature from 100-121oC over 20 minutes. Maintaina temperature of 121oC for 60 minutes ant then

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reduce the temperature from 121-100oC over 40 minutes, ventilationis done to prevent vacuum.
Remove the beaker from the autoclave.

Allow the ampoules to cool. Then wash these thoroughly to clear it off the dye. Visually examine
these ampoules in a white background.Seperate and discard those that do not contain clear solution.

Report:

Reference:

1. Indian Pharmacopoeia 2007,Volume-1, Published by The Indian pharmacopoeia commission,

Ghaziabad. Page no: 599-600.
2. Paul Abendroth, Robert N Clark, Glass containers for parenteral In Kenneth E Avis, Herbert A
Leiberman, Leon Lachman (es), Pharmaceutical dosage forms parenteral medications, volume -
1, 2rdedn, Marcel Dekker (1992), New york, Page no: 361 -369.

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Observation and calculation

Burette reading Volume of 0.01M

Titre volume
Initial Final HCl consumed (ml)

Test

Blank

Brimful volume =

90% average overflow volume =

Volume of 0.01M HCl actually consumed by the test solution =

Volume of 0.01M HCl consumed by test - Volume of 0.01M HCl consumed by blank

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Experiment No: 18
Date:
HYDROLYTIC RESISTANCE TEST FOR CONTAINERS

Aim: To perform hydrolytic resistance (water attack test) test for the given ampoules.

Requirements:Ampoules, distilled water, methyl red, 0.01M hydrochloric acid, autoclave, conical
flask, burette, measuring cylinder.

Principle: Glass is commonly used in pharmaceutical packing because it possesses superior protective
qualities. It is economical and readily available in variety of sizes and shapes. It is chemically inert,
impermeable, strong and rigid and has FDA clearance. Glass does not deteriorate with age and with
proper closure system, it provides excellent barrier against practically every element except light
coloured glass gives protection against light. Major disadvantages are its fragility and its weight.
Glass is composed principally of sand (silica),soda ash(sodium carbonate),cullet(broken glass that is
mixed with the batch and acts as fusion agent for the entire mixture).The common cations found in
glass wares are silicon, aluminium, boron, sodium, potassium, calcium, magnesium, zinc and barium.
The only anion of consequence is oxygen.
Since the surface of glass is an exposed oxide network, it can be reactive. On standing in contact with
aqueous solution alkali will leach out from it. This leaching is accelerated by heat, as occurs with
sterilization. The compendia specify the type of glass container to be used for certain materials and
include tests for four types of glass.

Based on components glass is grouped as follows:

Type I–Neutral glass is a borosilicate glass containing significant amount of boric oxide, aluminium
oxide, and alkali /alkaline earth oxides. It has high hydrolytic resistance. Suitable for all preparations
whether or not for parenteral use.
Type II– Soda lime treated glass; made of commercial soda lime glass that has been de-alkalized or
treated to remove surface alkali .Repeated exposure to sterilization and alkaline detergents will break
down the dealkalized surface and expose the underlying soda lime compound. They have high
hydrolytic resistance. Not suitable for parenteral use.
Type III– Soda lime glass, untreated. Moderate hydrolytic resistance.
Type IV– Soda lime glass, not suitable for parentrals.

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The USP and NF describe the various types of glass and provide the powered glass and water attack
test (hydrolytic resistance test) for evaluating the chemical resistance of glass. The test measures the
amount of alkalinity leached from the glass by purified water under controlled elevated temperature
conditions.

The powdered glass test is performed on crushed grains of a specific size which exposes internal surface
of the glass compound and water attack is conducted on whole containers and is used only for type II,
because of the dealkalanized surface. The results are based on the amount of alkali titrated by 0.01N
hydrochloric acid after an autoclaving cycle with the glass sample in contact with a high purity distilled
water.

Result is not greater than the value stated in the table.

Capacity corresponding to 90% Volume of 0.01M HCl per 100ml of test
avg.overflow volume (ml) solution (ml)

Type I or II Type III

More than 5,less than 10 1 10.2

Procedure: Rinse the ampoules twice with distilled water. Then fill the ampoules to the brim with the
distilled water, empty them and determine the average overflow volume. Again fill the ampoules with
the average overflow volume of distilled water and seal them by fusion method. Place the ampoules in
an autoclave, close the autoclave and displace the air by passage of steam for 10minutes, raise the
temperature from 100-121oC over 20 minutes. Maintain a temperature of 121oC for 60 minutes and
thenreduce the temperature from 121-100oC over 40 minutes, venting is done to prevent vacuum.
Removethe ampoules from the autoclave, cool in a bath of running tap water. Combine the liquids from
the ampoules.Measure out 50ml of the solution to the conical flask. Add 0.15ml of methyl red solution
to the conical flask and titrate with 0.01M hydrochloric acid. Repeat whole operation using the
sameamount of distilled water.

The difference between the titration represents the volume of 0.01M hydrochloric acid required by the
test solution.
Report:

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Observation and calculation

Burette reading Volume of 0.01M HCl

Initial Final consumed(ml)

Test

Blank

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Experiment No: 19
Date:
POWDERED GLASS TEST

Aim:To perform powdered glass (crushed glass) test for the given ampoules.

Requirements:Ampoules, distilled water, methyl red, 0.01M hydrochloric acid, autoclave, conical
flask, burette, measuring cylinder.

Principle:Glass is commonly used in pharmaceutical packing because it possesses superior protective

qualities. It is economical and readily available in variety of sizes and shapes. It is chemically inert,
impermeable, strong and rigid and has FDA clearance. Glass does not deteriorate with age and with
proper closure system, it provides excellent barrier against practically every element except light-
coloured glass gives protection against light. Major disadvantages are its fragility and its weight.
Glass is composed principally of sand (silica),soda ash(sodium carbonate), cullet(broken glass that is
mixed with the batch and acts as fusion agent for the entire mixture).The common cations found in
glass wares are silicon, aluminium, boron, sodium, potassium,calcium, magnesium, zinc and barium.
The only anion of consequence is oxygen.
Since the surface of glass is an exposed oxide network, it can be reactive. On standing in contact with
aqueous solution alkali will leach out from it. This leaching is accelerated by heat, as occurs with
sterilization.
The compendia specify the type of glass container to be used for certain materials and include tests for
four types of glass.

Based on components glass is grouped as follows:

Type I – Borosilicate glass, a substantial part of alcohol and earth cation are replaced by
barium/aluminium and zinc. Chemically inert and contain none or insignificant amount of cation.
Type II – Soda lime treated glass; made of commercial soda lime glass that has been de-alkalized or
treated to remove surface alkali. Repeated exposure to sterilization and alkaline detergents will
break down the dealkalized surface and expose the underlying soda lime compound.
Type III – Soda lime glass, untreated.
Type IV – Soda lime glass, not suitable for parenteral.

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 The USP and NF describe the various types of glass and provide the powered glass and water
attack test (hydrolytic resistance test) for evaluating the chemical resistance of glass. The test measures
the amount of alkalinity leached form the glass by purified water under controlled elevated temperature
conditions.
The powdered glass test is performed on crushed grains of a specific size which exposes internal
surface of the glass compound and water attack is conducted on whole containers and is used only for
type II, because of the dealkalized surface. The results are based on the amount of alkali titrated by
0.01N hydrochloric acid after an autoclaving cycle with the glass sample in contact with a high purity
distilled water.
Procedure: Rinse thoroughly with purified water six or more ampoules at random and dry them. Crush
the containers into fragments with pestle and empty the mortar into no: 20 sieve. Shake the sieves for
a short time. Remove glass from no: 20 and no: 40 sieve and again crush and sieve as before. Transfer
the portion retained on no: 50 sieve, which should weigh in excess of 10g to a closed container.
Transfer 10g to 250ml conical flask. Add 50ml high purity water to this flask and to one similarly
prepared to provide a blank.Place it in autoclave. Close the autoclave and displace the air by passage
of steam for 10minutes, raise the temperature from 100-1210C over 20 minutes. Maintain a temperature
of 1210C for 60 minutes and then reducethe temperature from 121-100o.Cover it for 40 minutes, venting
is done to prevent vacuum. Remove the flask from the autoclave.
Cool the flask in running water, decant water from the flask into cleansed vessel and wash the
residual glass with four 15ml portions of high purity water, add decanting to the main. Add 0.15ml of
methyl red solution to the conical flask and titrate with 0.01M hydrochloric acid.
Report:

Reference:
1. Indian pharmacopoeia 2007, Volume-1, published by The Indian pharmacopoeia commission,
Ghaziabad, Page no: 599-600.
2. Paul Abendroth, Robert N Clark, Glass containers for parenterals In Kenneth E Avis, Herbert A
Leiberman, Leon Lachman, Pharmaceutical dosage forms parenteral medications, volume - 1, 2rd
edition, Marcel Dekker (1992), New York, Page no: 361 -369.

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 OPHTHALMIC PREPARATION

Ophthalmic products are the sterile products meant for instillation in to the eye in the space
between the eyelids and eyeballs. These products are sterile and prepared under the extreme conditions
and by the same method as the other parenteral preparation. Essential characteristics of different
ophthalmic preparation should posses the following properties.

Foreign particles: All the ophthalmic products must be clear and free from foreign particle, fibers and
filaments. The particle size of the eye suspension should be in ultra fine state to minimize the irritation.

Viscosity:In order to prolong the contact time of the drug in the eye, thickening agents are added in to
the preparation.

Isotonicity: It must be isotonic with the lachrymal secretions to avoid discomfort and irritation. It has
been observed that eye can tolerate in the range of 0.5 to 2 % sodium chloride.

pH of the preparation:pH of the preparation plays an important role in the solubility stability and
comfortness of the product.

Sterility: The ophthalmic product prepared must be sterile.

References:Pharmaceutics practical manual by Dr. P Muthuprasanna, Page no: 23.

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Observations and calculations

Specimen Label

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Experiment No: 20
Date:
SODIUM BICARBONATE EYE LOTION

Aim: To prepare and submit 30 ml of sodium bicarbonate eye lotion.

Ingredients: Sodium bicarbonate, purified water.

Principle:Ophthalmic preparations are sterile dosage forms essentially free from foreign particles or
viable micro organisms suitably compounded or prepared for the easy administration. Eye drops are
aqueous or oily suspension instilled in to the eye cavity place between eyelid and eye ball and carry
anti microbial, anti inflammatory anti allergic and smoothening drug for local action.

Procedure: Dissolve sodium bicarbonate in small quantity of water and make up the solution to the
required volume by adding more water. Sterilize by autoclaving.

Storage: Store in a dry and cool place.

Report:

Reference:Pharmaceutics practical manual by Dr. P Muthuprasanna, Page no: 24.

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Observations and calculations

Specimen Label

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Experiment No: 21
Date:
ZINC SULPHATE EYE DROPS

Aim: To prepare and submit 20ml Zinc sulphate eye drops.

Formula
Zinc sulphate – 3 mg
Sodium chloride- 40 mg
Solvent for eye drops – up to 15 ml

Principle: Ophthalmic preparations are sterile dosage forms administered in eye, which are essentially
free from foreign particles or viable micro organisms suitably compounded or prepared for the easy
administration. Eye drops are aqueous or oily suspension instilled in to the eye cavity place between
eyelid and eye ball and carry anti microbial, anti inflammatory,anti allergic and smoothening drug for
local action. Zinc sulphate used in this eye drop is colourless, transparent crystal having astringent
activity.Zinc sulphate eye drops are used as astringent.

Procedure: Dissolve weighed quantity of zinc sulphate in water (purified water) with aseptic
precautions. Add sodium chloride to it and if required filter it aseptically.

Use: Anti-infective.

Use: Astringent.

Dose: 1-2drops

Storage: Stored in a well closed container

Auxiliary label:Not for internal use.

Do not touch the dropper tip

Report:

Reference: Pharmaceutics practical manual by Dr. P Muthuprasanna, page no: 22.

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Observations and calculations

Specimen Label

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Experiment No: 22
Date:
BORIC ACID EAR DROPS

Aim: To prepare and submit boric acid ear drops.

Formula
Boric acid – 0.2 g
Specially denatured spirit – 3 ml
Purified water sufficient to produce - 15 ml

Principle: Ear drops are liquid preparation suspensions, emulsions or solution of one or more
medicament in a vehicle suitable for instillation in to the ear. Ear drops should be supplied in the
container with dropper. Boric acid ear drop is used as anti infective.Ear drops carry anti microbial, anti
inflammatory, anti allergic and dewaxing agents.

Procedure:Dissolve weighedquantities of boric acid in denatured spirit and add purified waterup to 15
ml. If any impurities are present filter it. Dispense in suitable container.

Use: Anti-infective.

Dose: 3– 5 drops

Storage: Stored in a well closed container.

Auxiliary label:Not for internal use

Do not touch the dropper tip

Report:

Reference:Pharmaceutics practical manual by Dr. P Muthuprasanna, Page no: 23.

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 SUSPENSIONS

Suspensions are biphasic liquid dosage form of medicament in which finely divided solid particles
ranging from 0.5 to 5.0 micron are suspended or dispersed in liquid or semisolid vehicle.

Qualities of good suspension

 Particles dispersed should not settle down rapidly and should re-disperse on shaking.
 Particles should not form a cake.
 Viscosity should be optimum.
 They should be chemically stable.

Suspensions are of two types Flocculated and Non Flocculated suspensions.

In flocculated suspensions, the particles form loose aggregates and form a network like structure where
as in non-flocculated system they do not. Rate of sedimentation is high in flocculated suspension
whereas in non- flocculated it is very low. In flocculated suspension, the particles are loosely packed
and do not cake whereas in non-flocculated the particles are closely arranged and they form a cake.
Flocculated suspensions are easy to re-disperse where as non-flocculated are not. Flocculated
suspensions do not give a pleasing appearance whereas non-flocculated give a pleasing appearance as
the floccules do not stick to the sides of the container where as in flocculated they do.

Formulation: Suspensions mainly contain;

 Flocculating agent: which ensure particles are well dispersed in the vehicle Eg: Tweens, spans etc.
 Suspending agents: They are added to increase the viscosity of continuous phase so that particles
remain suspended for long time.Eg: Sodium CMC, HPMC, MC, CMC.
 Wetting agents: They are added to reduce the interfacial tension between solid and liquid medium
producing suspension of desired quality. Eg: Glycerine, Tragacanth, glycols, polysorbates.
 Dispersing agents: They increase the zeta potential on the particles of the suspensions and do not
allow the particles to settle down. Eg: Stearates.
 Preservatives: They are added to prevent microbial growth in the suspensions.
Eg: Sodium benzoate, Methyl and propyl parabens.
 Organoleptic additives: They are added as colours, flavours and sweetening agents.

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Experiment No: 23
Date:
FORMULATION OF ANTACID SUSPENSION & DETERMINATION OF ITS ACID
NEUTRALIZING CAPACITY

Aim:To formulate and evaluate antacid suspension to estimate its acid neutralizing capacity.

Method: Formula of Antacid suspensions

Ingredients Quantity / 100 ml

Aluminium hydroxide gel I.P 3g
Magnesium hydroxide I P 1.25 g
Sorbitol 25mg
Sodium CMC 2g
Peppermint oil q.s
Purified water q.s. to 100 ml

Principle: Pharmaceutical suspension is a coarse dispersion in which internal phase is dispersed

uniformly throughout the external phase. The internal phase consisting of insoluble solid particles
having a specific range of size which is maintained uniformly throughout the suspending vehicle with
aid of single or combination of suspending agent.

Antacids are drug products which on oral administration neutralize excess gastric acid and
lower the acidity of gastric contents. Antacids are used widely for the relief of heart burnand dyspepsia,
and other nonspecific gastrointestinal symptoms.Combinations of Mg2+ (rapidly reacting) and Al3+
(slowly reacting) hydroxides provide a relatively balanced and sustained neutralizing capacity. Both
magnesium hydroxide and aluminum hydroxide react with excess acid in the stomach thereby
neutralizing gastric acid. The potency of an antacid is generally expressed in terms of its Acid
neutralizing capacity (ANC). ANC is defined as the number of milliequivalents (mEq) of 1N HCl that
is brought to a pH of 3.5 in 15 minutes by a unit dose of an antacid preparation. Chemical composition,
nature of drug particles and rheology of suspension influences the ANC.

Sodium CMC acts as a suspending agent. Sorbitol is the sweetening agent and peppermint oil
acts as flavouring agent.

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Formulation:

1. Take about 30 ml of purified water in a beaker and dissolve sorbitol in it.

2. DissolvePeppermint oil in alcohol and add to the sorbitol solution with agitation.
3. Pass Aluminium hydroxide gel and Magnesium hydroxide through sieve no.40 and make into a
paste with the sorbitol solution using a mortar and pestle.
4. Soak Sodium CMC/sodium alginate in 25 ml water and carefully homogenize using a stirrer.
5. To this viscous vehicle addthe above mixture and homogenize the solution using a stirrer.
6. Then transferthe above contents in to a measuring cylinder andmake up the final volume to 100 ml
with purified water.

Determination of Acid neutralizing capacity:Treatexcess acid with a known quantity of antacid.

After the neutralization reaction determine the excess of the acid remaining by titrating against 0.5N
sodium hydroxide. Determine the end point by noting the pH of the reaction media i.e. 3.5 pH should
be maintained for 10-15 seconds.

1. Determined the density of the antacid preparations using specific gravity bottle.
2. Transfer weight equivalent to 5ml of each antacid solution into a 250ml beaker. Make upthe volume
to 70ml with distilled water and mix for a minute using magnetic stirrer.
3. Add30ml of 1N hydrochloric acid into the above solution & mix well for 15 minutes.
4. Titrate the excess acid against 0.5N sodium hydroxide within 5min. The volume of sodium
hydroxide consumed for bringing the pH to 3.5, which maintained for 10 – 15 sec is noted using a
digital pH-meter.
5. The number of mill equivalents (mEq) of acid consumed per ml of the test substance is then
calculated.

Report:

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 CREAMS

Creams are viscous semisolid preparations or emulsions which are meant for external use. Creams are
those emulsions which are either oil in water or water in oil type. Depending on the main ingredients
and use, they are broadly classified in to

1. Make-up creams (o/w type emulsions)

- Vanishing creams
- Foundation creams
2. Cleansing creams (w/o type emulsions)
3. Creams for winter
- Cold cream
4. Creams for dry skin
- Moisturizing creams
5. All purpose cream
6. Night creams
7. Skin protective and hand cream

FORMULATION:

 Water: Pure water is used in creams.

 Oil, fat and waxes: Eg: paraffin wax, ozokerite and ceresin.
 Humectants: Eg:Ethylene glycol, Diethylene glycol.
 Emulsifying agents: Eg: Gum tragacanth, Methyl cellulose.
 Alkalies: Borax, NaOH, K2CO3
 Perfumes: essential oils, floral extracts.

References:Cosmetic technology by Sanju Nanda and Arun Nanda, 2009, 1st edition, Page no: 244-
249.

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Observations and calculations

Specimen Label

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Experiment No: 24
Date:
COLD CREAM

Aim:To prepare and submit 20 g of cold cream.

Formula: Bees wax 20g

Borax 1g
Purified water 19g
Liquid paraffin 60g
Principle:The term cold is due to cooling sensation caused by evaporation of water in cream after it is
applied to the skin. It is a w/o emulsion that is made by using bees wax and alkali.The cream contains
high percentage of mineral oil for cleansing efficacy. Basically they are o/w type emulsion. After
rubbing to the skin sufficient quantity of water evaporates to impart a phase inversion to w/o type. The
solvent action of the oil imparts the cleansing property.In this bees wax – borax type preparation, borax
react with the free fatty acid present in bees wax and produce soft soap which acts as emulsifying agent
and emulsifies the oil phase containing bees wax, mineral oil, paraffin etc. in the aqueous phase.

Procedure:Melt bees wax in awater bathto about 70oC add light liquid paraffin to it. In anotherbeaker
heat water to about 70oC and dissolve borax in it.Mix aqueous phase to the oily phasewith stirring till
a creamy emulsion is prepared. Add perfume at about 40oC. Allow to cool to room temperature. Fill in
the suitable container and label.

Storage:Store in a cool dry place at a temperature not exceeding 25°C. Do not freeze.

Use:Emollient and protective in dry skin condition.

Report :

Reference: Cosmetic technology by Sanju Nanda,Arun Nanda, Page: 250.

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Specimen Label

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Experiment No: 25
Date:
VANISHING CREAM

Aim: To prepare and submit 20g of vanishing cream.

Formula: Stearic acid 18g

Potassium carbonate 1g
Glycerine 5g
Water 76 ml

Principle:Vanishing creams are so called because they seem to disappear when rubbed into the skin.
These preparations are stearic acid based o/w type emulsion. A part of stearic acid is saponified with
an alkali and rest of stearic acid is emulsified with this soap in large quantity of water. After application
cream leaves a dry but tacky residual film which also has a drying effect on the skin. These creams can
be quickly washed off with water due to o/w nature.

Stearic acid is the main ingredient which provides apearly white shining appearance to cream.
Characteristics of the cream vary according to the proportion of stearic acid, total proportion should
not exceed 25% and best proportion should not exceed 16-20%. The consistency and texture of cream
depends on the amount of acid saponified and nature of alkali used. Alkalies normally used are
triethanolamine, borax and ammonia. Glycerin maintains the consistency and enhances spreadability.

Procedure:Melt stearic acid by indirect heat in a water bath. Dissolve potassium carbonate in water
and add glycerin.Heatthis to about 75oC and slowly add to the melted stearic acid with constant stirring
until a smooth homogenous cream is formed. Cool to 45°C, add perfumes at about 40oC and pack in
suitable container.

Storage: Store in a cool dry place below 25°C. Do not freeze.

Use:Cosmetic cream base, as a foundation for makeup.

Report :

Reference: Cosmetic technology by Sanju Nanda and Arun Nanda Page no: 253.

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Observations and calculations

Specimen Label

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Experiment No: 26
Date:
FOUNDATION CREAM

Aim: To prepare and submit 20 g of foundation cream.

Official Formula:
Lanolin 2%
Cetyl alcohol 0.45%
Stearic acid 10%
Propylene glycol 8%
KOH 0.4%
Water 79.17%
Perfume qs
Purified water qs

Principle:Foundation creams areapplied to skin to provide a smooth emollient base or foundation

before the application of face powder or other preparation on face.These are variants of vanishing cream
formulae.They help the face powder to adhere to skin due to good holding power. They should spread
well, non-greasy, should leave non occlusive layer on face.The foundation cream can be of 2 types.
1. Pigmented cream which are coloured
2. Impigmented cream

Procedure: Heat the ingredients of oil phase such as lanolin, cetyl alcohol and stearic acid and aqueous
phase ingredients such as propylene glycol, potassium hydroxide and water separately at 750 Cand mix
the aqueous phase to oil phase slowly with continuous stirring. Add perfume when temperature is about
40ºC. Preservative should be added to water before mixing with oily phase. Cool while stirring.
Transfer to container and label and dispense.

Use: Foundation formakeup.

Storage: Store in a cool place.

Auxiliary Label: FOR EXTERNAL USE ONLY

Report :

Reference: Cosmetic technology by Sanju Nanda and Arun Nanda, Page no: 254

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Specimen Label

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FINAL BPHARM, NATIONAL COLLEGE OF PHARMACY
Experiment No: 27
Date:
ALL PURPOSE CREAM
Aim:To Prepare and Submit 20 g of All Purpose Cream
Formulation:
Stearic acid 12%
Lanolin 4%
Emulsifying wax 5%
Mineral oil 29%
Tween 80 1%
Glycerine 10%
Water qs 100ml
Perfume qs
Preservative qs
Antioxidant qs
Principle: Any cold cream may be called as cold cream ;they are oily but not greasy type and but can
spread easily on the skin to give a protection film. They can also function as nourishingcream, night
cream and aprotection cream. It is also used for prevention of sunburn and for treatment of roughed
skin areas. The composition of the cream can act as foundation cream to provide a foundation base and
for makeup as acleansing cream. As a hand cream and should have emollient character.
Procedure: Melt required quantity of stearic acid, lanolin, emulsified wax and mineral oil at about
750C. Separately heatthe glycerin and water to the same temperature. Add oil phase to aqueous phase
with constant stirring. Add perfume and obtain a homogenous smooth cream.
Use:Emollient, cleansing and protective.

Report:

Reference:Cosmetic technology by Sanju Nanda and Arun Nanda, Page no: 269.

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 POWDERS

Facepowder is a cosmetic preparation which has its prime function to compliment skin colour by
imparting a velvet finish to face. The powder must be able to produce lasting effect. It should make the
face pleasant to touch and look. It masks visible imperfections of the face and make the skin shiny.

Characteristics:The material selected shall have one of the following properties;

a) Covering powders:The purpose of this is to conceal defects like scar, blemishes, and enlarged
pores & gives excessive shining on the skin.

Eg: Titanium dioxides, kaolin, zinc oxide.

b) Absorbing powders:This eliminates shiny skin by absorbing sebaceous secretion and

perspiration. Kaolin, Magnesium carbonates.
c) Slip:Quantity of easy spreading and application of powder to produce smoothness on the skin.
Eg: Talc,Metallic soap.
d) Adhesion: They impart adhesion character not only to the skin but also to the powder puff. Eg.
Talc magnesium stearate.
e) Bloom: It is the ability to impart velvety peach like finish to the skin. Eg: Chalk, prepared
starch.
f) Colouring organic or organic pigments: Organic cakes, water or oil soluble die salts are
seldom used.

Classification:

1. Light type: Dark skin requires light powder; they contain large quantity of talc.
2. Medium type: They have coloring powder used for moderate or medium skin
3. Heavy type: High coloring powder used for oily skin.

Reference: Cosmetic technology by Sanju Nanda and Arun Nanda, Page no: 257

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FINAL BPHARM, NATIONAL COLLEGE OF PHARMACY
Experiment No: 28
Date:
FACE POWDER
Aim: To prepare and submit 10 g of face powder.
Official Formula:
Talc 39.5%
Kaolin 39.5%
Chalk precipitate 10%
Magnesium stearate 5%
Zinc oxide 5%
Perfume qs
Colour qs

Principle: Function of face powder includes imparting smoothness to the skin, masking of minor
visible imperfections of skin, and masking of shine due to moisture or grease. It should look natural,it
should have lashing properties, and it should be reasonably resistant to undesired reactions and should
serve as a vehicle for perfume to be incorporated. To achieve these, powder should have covering
powder,grip,absorbency,adhesiveness and bloom.

Procedure:Separately sievethe dry ingredients. Add perfume along with the part of the calcium
carbonate and keep aside. Mix the ingredients together to obtain a uniform powder mixture. Sieve the
powder mixture using a mesh. Transfer it into a suitable container. Pack and label.

Use: Used as face cosmetic

Report :

Reference:Hand book of cosmetics by B. M Mithal. Page no: 26.

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Experiment No: 29
Date:
COMPACT FACE POWDER
Aim: To prepare and submit 10 g of compact face powder.
Official Formulae
Talc -55%
Magnesium stearate -5%
Calcium carbonate -5%
Zinc oxide -15%
Kaolin -15%
Titanium dioxide -3%
Perfume -q.s
Binary formulae
Gum acacia -1g
Glycerin -5g
Water -94g
Principle: The compact face powder is a dry powder which has been compressed into a cake,and is
initially applied with a powder puff. The composition of compact powder is more or less same as that
of loose powder. The material of compact face powder must compress easily and remain compact,not
to break under normal condition of use. At the same time the powder must adhere easily to powder
puff. In the binder solution, glycerol and acacia are used. Acacia act as water soluble binder. Glycerol
acts as an emulsion binder and humectant.
Procedure: Separately sieve all dry ingredients.Addperfume with a part of adsorbent Calcium
carbonate and keep aside. Mixother ingredients together and finally a uniform powderedmixtureis
obtained.Sieve this using mesh or washed nylon cloth. Mix the binder solution with the above mixture
to make an adherent mass.Compress the mass in a container and heat it on an oven.
Category: Protective.
Storage: Stored in a well closed container.

Report :

Reference:Hand book of cosmetics by B. M Mithal. Page no: 30.

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Experiment No: 30
Date:
PRICKLY HEAT POWDER

Aim: To prepare and submit 10 g of prickly heat powder.

Official Formulae:
Menthol -2g

Salicylic acid -10g

Zinc oxide -284g

Talc -300g

Starch -400g

Camphor -4g

Principle: In this powder preparation, menthol and camphor are used for their antipruritic action.Zinc
stearate or oxide is a dissociative and protective agent.Starch is used to dissolve the moisture.Talc is
used as rubefaciant. Camphor and menthol also provide cooling effect.

Procedure:Take menthol and camphor together.Add mixture of zinc oxide and salicylic acid, mix
thoroughly by adding talc and finely incorporated with starch.Pass resulting powder through sieve no:
120.

Storage:Store in a well closed container in a cool and dry place.

Use: Antipruritic

Report :

Reference:Hand book of cosmetics by B. M Mithal. Page no: 33.

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Specimen Label

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FINAL BPHARM, NATIONAL COLLEGE OF PHARMACY
Experiment No: 31
Date:
POWDER ROUGE

Aim: To prepare and submit 10g of dry rouge.

Official Formulae:
Talc -2.4g
Kaolin - 0.8g
Chalk -0.2g
Magnesium carbonate -0.2g
Zinc stearate -0.2g
Titanium dioxide -0.6g
Rose oil -q.s
Colour -q.s

Principle: Rouge is makeup formulation or foundation preparation used along with powder .Kaolin
used in this preparation to provide binding property.Talc provides a covering property.Chalk provides
the brushing of rouge.Titanium dioxide is usedas an agent.Zinc stearate provides a flexible film over
the skin.Rose oil is inclined for the perfuming action.

Procedure:Add perfume with magnesium carbonatemixed properly and keep it covered for half an
hour.Mix the remaining powder thoroughly and sieve through fine muslin.Add magnesium carbonate
and then the required colour.Mix thoroughly and store in suitable container.

Use:Facial make up

Report :

Reference: Hand book of cosmetics by B. M Mithal. Page no: 50.

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 SHAMPOO

They are defined as the preparation of the surfactant in a suitable form liquid, solid or powder which
when used under the conditions specified will remove surface grease, dirt and skin debris from the hair
shaft and scalp without affecting adversely the hair, scalp and health of the user. A shampoo
formulation may be compounded to emphasis some specialized capabilities like minimizing eye sting,
controlling dandruff or imparting appealing fragrance to gain a more favorable acceptance. It should
not remove too much of natural oil from the scalp. The success of shampoo is replacing the coke of
soap lies in the fact that the shampoo is not only a detergent but as cosmetic as well as it must impart
luster, beauty, soft fragrance and manageability. Shampoo is available in variety forms such as clear
liquids, lotions, paste, gel, aerosol and dry products.

Raw materials:
Soap: defined as salts of fatty acids obtained by saponifying material animal and vegetable fat and oil
with alkali such as sodiumhydroxide and potassium hydroxide.
 Synthetic detergents: Developed by replacing the -COOH group linked to end of long chain
hydrocarbon in soaps and as classified by the nature of their hydrophilic groups.
 Amphoterics:Ionized but the polarity of the charge depends up on solution pH.

Shampoo additives
 Foam builders: Added to increase the quality, volume, viscosity, stability and also promote slight
conditioning effect to the hair. Eg: lauryl mono ethanol amine.
 Conditioning agent: Foam a thin coating over the hair. Improve the handling character of the
hair fiber. Eg: glycerol, isopropyl palmitate.
 Opacifying agent:Eg: Steryl ethyl alchohol.
 Clarifying agent: Helps to maintain shampoo clarity through over wide range of temperature.
They should be checked for eye irritation. Eg: terpiniol, di ethylene glycol.
 Sequestering agent: Added to prevent the formation of insoluble calcium and magnesium salts
when the shampoo is mixed with hard water. Eg: Citric acid, EDTA.
 Anti-dandruff agents:Eg. sulphur salicylic acid.
 Thickening agents: Natural gum: Tragacanth, Gum acacia.

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  Preservatives: Methylparaben and propylparaben.
 Other stabilizing agents:Anti oxidants: protect from discoloration due to oxidation
Suspending agents: it is used in the case of insoluble products
pH control agents: protect the product due to change in the pH.

Reference:Cosmetic technology by Sanju Nanda and Arun Nanda, Page no: 354

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Specimen Label

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Experiment No: 32
Date:
CASTOR OIL SHAMPOO

Aim: To prepare and submit 20ml of castor oil shampoo.

Formula: Castor oil 16 ml
Potassium hydroxide 5g
EDTA 100 mg
Boric acid q.s
Perfume q.s
Water q.s to 100 ml

Principle:These are liquid shampoos containing potassium soaps because of the greater solubility.
They are protected with sequestering agents such as EDTA which hinder the formation of calcium and
magnesium salt, when these ions are introduced via hard water. They are made from oils and known as
oil shampoos. Boric acid is added to maintain pH at 8.5.

Procedure:Heat oil and potassium hydroxide on a water bath until saponification is completed and
soap is formed. Dissolve soap in sufficient quantity of water; add boric acid until pH is 8.5. Add EDTA
and make up the volume.

Container:Pack in plastic bottle made of polyvinyl chloride and polyethylene.

Labeling:Wet the hair, massage onto scalp, lather and rinse thoroughly. Avoid contact with eyes.If this
happens, rinse thoroughly with water.

Storage:Store in cool place, protect from light, keep out of reach of children.

Use:For cleansing hair and shaft.

Report :

Reference: Cosmetic technology by Sanju Nanda and Arun Nanda, Page no:367

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Specimen Label

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FINAL BPHARM, NATIONAL COLLEGE OF PHARMACY
Experiment No: 33
Date:
COCONUT OIL SHAMPOO
Aim:To prepare and submit 20ml of coconut oil shampoo.
Formula: Coconut oil 16 ml
Potassium hydroxide (85%w/v) 5.3 ml
EDTA 100 mg
Boric acid q.s
Purified water q.s to 100 ml
Principle:The oils containing shorter chain fatty acid such as coconut oil yield better foaming soaps
with potassium hydroxide because of its solubility. Shampoos based on coconut oil do not perform well
in hard water area. They lather poorly and have a tendency to deposit dulling film of insoluble calcium
and magnesium salts on the hair. This is corrected by addition of sequestering agents such as EDTA.
Boric acid is added to adjust until pH is 8.5.

Procedure:Heat oil and potassium hydroxide on a water bath to form soap. Dissolve soap in water.
Adjust pH by the addition of boric acid to 8.5. Place the mixture in refrigerator for chilling, then remove
the creamy (unsaponified matter) layer. Filter and fill in a shampoo container.

Container:Pack in plastic bottle made of polyvinyl chloride and polyethylene.

Labeling:Wet the hair, massage onto scalp, lather and rinse thoroughly. Avoid contact with eyes. If
this happens, rinse thoroughly with water.

Storage:Store in cool place, protect from light, keep out of reach of children.

Use:For cleansing hair and shaft.

Report :

Reference:

1. Cosmetics science and technologyby M.S Balsam and Edward Sarg, second edition, Vol-II, Page
no: 84-86.
2. Cosmetic technology by Sanju Nanda and Arun Nanda, Page no: 360.

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 SHAVING PREPARATIONS

Products employed by men primarily to help in shaving.Shaving preparation basically classified in to

two types.

1. Preparation used before shaving.

2. Preparation used after shaving.

Shaving preparation are further classified in to

1. Shaving soap cream
2. Brushless shaving cream.
3. Aerosol preparations.

Shaving soap cream

They are applied prior to shaving in order to wet and soften the beard. The foam they produce help to
hold the hair erect for cutting. They are of lathering type are basically composed of sodium or potassium
stearates.

Brushless shaving cream

They are oil in water type emulsions. The difference is that the level of oil and fatty acid tent to be
higher. They give more compatible shave as they soften the beard more thoroughly. They have a pH of
7.5 to 8.5.and cause less irritation on broken skin.

Aerosol preparations
They are oil in water type emulsions. Here aerosols can easily be filled with soaps solutions and
concentrated tighter with propellant added under pressure.

AFTER SHAVE PRODUCTS

These are preparation intended to cool and refresh the skin and exert mild astringent effect. They also
protect from the bacterial infection. The most popular type of after shave lotion is clean lotion
containing 50-70% ethanol and appropriate level of water. They reduce the skin irritation due to minor
cuts and effect of chemicals used in shaving preparation.

Reference: Cosmetic technology by Sanju Nanda and Arun Nanda, Page no: 418.

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Specimen Label

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FINAL BPHARM, NATIONAL COLLEGE OF PHARMACY
Experiment No: 34
Date:
SHAVING SOAP CREAM
Aim:To prepare and submit 50g of shaving soap cream
Formula:
Stearic acid 30g
Coconut oil 10 g
Palm oil 5 gm
Potassium hydroxide 7 gm
Sodium hydroxide 1.5gm
Water 36.5g
Glycerin 1.5 g
Gelatin qs
Perfume qs
Preservative qs
Principle:Shaving cream is applied prior to shaving to wet and soften beards.Thefoam they produce
help to hold the hair erect for cutting.Shaving cream preparation of lathering types are basically soaps
composed of potassium stearate mixed with water and glycerol to give a creamy soft texture. In this
preparation a mixture of 75% stearic acid with 25 % coconut oil is used.
Procedure:Heat oil phase and aqueous phase to a temperature of 70oC.Incorporate preservative with
glycerin in water. Add oil phase in aqueous phase with constant stirring, cool to 45oCand add perfume.
Fill in the container and label.

Report :

Reference:Cosmetic technology by Sanju Nanda and Arun Nanda, Page no: 421

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FINAL BPHARM, NATIONAL COLLEGE OF PHARMACY
Experiment No: 35
Date:
AFTER SHAVE LOTION

Aim:To prepare and submit 20 ml of after shave lotion.

Formula:
Ethyl alcohol (specially denatured) 50%

Sorbitol 70% solution 2.5%

Perfume 0.5%

Menthol 1.0%

Boric acid 2.0%

Purified water 44.9%

Principle:After shave preparations are intended to cool and refresh the skin and exert mild astringent
effect. They also protect from the bacterial infection.It is a clear alcoholic solution.Ethyl alcohol when
employed at right concentration in an after shave lotion mild astringency and refreshing coolness that
is unique. Mild acids such as boric acid are used to correct the alkaline reaction.Sorbitol acts as
humectants. It can be replaced with glycerol if more active humectants are desired or with propylene
glycol if a less residual film is preferred. Combination of 2 or more humectants is useful to obtain effect
not possible with single humectants. Menthol provides a cooling effect. The percentage of perfume will
depend on the type of perfume oil used.

Procedure:Dissolve all the ingredients in alcohol and dilute with water by agitation. Allow to stand
for chilling until the poorly soluble constituents of perfume oil have agglomerated. Then filter the
solution. If the lotion is to be coloured, add colour to the clarified solution. After it has warmed back
to the room temperature re-filter without further chilling to obtain brilliant polish nature.

Use: Used as an astringent and for providing cool and refreshing effect of after shaving.

Report :

Reference:Cosmetic technology by Sanju Nanda and Arun Nanda page no: 435.

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 LIPSTICK

Lipstick is a cosmetic preparation used for the modification of lip colour and the enhancement of facial
makeup. It is prepared by moulding a dispersion of colour in a waxy base in the form of a stick or
crayon fitted in a swirl cup. Lipstick provides a convenient means of either freshen the makeup to
colouring or protection of the lips from affects of cold or dry weather.

Formulation:

 Solid waxes: a) Common wax. Eg. Bees wax

b) Micro crystalline wax. Eg. Ceresine
c) Hard waxes. Eg.Carnauba
 Softening agent : Petrolatum, wool fat,lanolin, cocoa butter, lecithin
 Liquid components: Castor oil, mineral oil, vegetable oil
 Colour system: Soluble colour.Eg. dyestuffs
Insolublecolour. Eg. Staining dyes
Pigments:organic and in organic pigments.
Lakes: Aluminium lakes.Eg.F D & C Red No 3, D & C Red No 21

Miscellaneous agents

 Preservatives: Eg. Propyl Para hydroxyl benzoate

 Anti oxidants: Eg. Citric acid, BHT(butylated hydroxyl toluene)
 UV filters: Eg. benzophenon,titanium dioxide
 Flavours: Eg. Fruity flavours

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Specimen Label

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Experiment No: 36
Date:
LIP STICK

Aim: To prepare and submit 10 g of lipstick.

Official Formula:
Carnauba wax -1g
Bees wax -1.5g
Lanolin -0.5g
Cetylalcohol -0.5g
Castor oil -6.5 ml
Colour -q.s

Principle: It is composed of essentially of an oil-wax base stuff enough to form a stick with staining
dye dissolved or dispersed in the oil and pigments suspended there in suitably perfumed and flavoured,
moulded and enclosed in a case. Here carnauba wax, Bees wax castor oil and lanolin together used as
lipstick base. Lanolin improves the covering property of the lipstick and also in the dispersion of the
colour. Cetyl alcohol is used as the solvent. Bees wax gives structure to the lipstick; keep it solid even
in warm climate. Perfumes cover the fatty odour present in the base. Here amaranth solution is used as
colouring agent.

Procedure: Melt carnauba wax,beeswax,cetyl alcohol and lanolin. Then disperse castor oil,add colour
and mix well till a homogenous mass is formed. Pour this mixture to a lipstick mould previously coated
with castor oil and cool for solidify.

Use: Lip cosmetic

Report :

Reference: Cosmetic technology by Sanju Nanda and Arun Nanda, Page no: 331

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Observation and calculation

Specimen Label

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Experiment No: 37
Date:

NAIL LACQUER

Aim: To prepare and submit 5 ml of nail lacquer.

Official Formulae: Nitrocellulose – 250 mg

Amylacetate -3.5 ml
Acetone -q.s to10 ml

Theory: Nail lacquers are viscous preparations intended to decorate nails of fingers and toe.A nail
lacquer or enamel contain a film whose characteristics are ease of brushing application,ease of drying
and hardening and whose formulation should enhance adhesion to nail without loosing its resistance to
chipping and abrasion. They can be transparent or coloured plain or with a glitter but they should
provide a smooth,impervious film as the nail without leaving any stain on its surface.The constituents
of nail lacquer are as follows:

Primary film formers

Secondary film forming resin
Plasticizers
Solvent
Colourant
Speciality filters

Formulation:A nail lacquer consists of colourants in lacquer base and other formulating agents added
to it.

1. Lacquer base include film formers, resin, plasticizer, solvent and diluents
2. Colouring agent involves dyes/lakes, pigments, glitters, pearlescent agents.
3. Other formulating agents consist of opacifying agents, suspending agents.

Film formers include nitrocellulose,cellulose acetate butyrate,ethylcellulose,vinyl polymers and

various polymers of methacrylate.Nitrocellulose is most acceptable.There are different types of
nitrocellulose as RS,AS and SS.RS has 11.8-12.2% nitrogen content which is used for nail lacquer

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formulation.Resins are used in conjugation with nitrocellulose composition to improve the degree of
film build and also to promote better glass and adhesion.

Natural resins – dammar, shellac

Synthetic resins – polyvinyl acetate,butyrate and arylsulphonamide,HCHO resins
Plasticizer- Impart flexibility and adhesive properties to the skin.They are solvent plasticizer-butyl
acetyl recinolate.

Non solvent plasticizer: Dibutyl phthalate

1. Active solvents: Liquids that dissolves nitrocellulose

Eg: ketone,esters,amides,glycol,ethers and nitroparaffins
2. Couplers or latent solvents: Generally alcohol themselves are not solvent for nitrocellulose but
when used in conjugation active solvents they increase the strength of latter.
3. Diluents: Non solvents for nitrocellulose. They are used to stabilize the viscosity in nail lacquer.
4. Colourants – They must be FDA certified,organic red pigments include litholrubines,lithol and
tobbiomaroon.Inorganic pigments are cosmetic grades of yellow and red
oxides,ironblue,ironblack,carbon black and purified titanium dioxide.Soluble dyes should not
be used.

Pearlescent materials like crystalline guanine in nitrocellulose are also incorporated.

Suspendingagent:Benzyldimethylhydrogenatedtallow,dimethyldioctyldecylammoniumbentonite.

Procedure: Dissolved nitrocellulose in amyl acetate.Made up to volume with acetone

Use: For decorating nail

Report :

Reference: Cosmetic science and technology, II edition by M.S Balasam and Edward sagarin, page
no:592.

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 ORAL PREPARATIONS

They are meant to clean teeth and other parts of oral cavity. They Include Toothpaste, Tooth powder,
Dental foams and dental creams.

Toothpaste: Semisolid preparations containing a very high percentage of solid particles and meant to
clean the surface of teeth with the help of a tooth brush. They enhance the personal appearance of the
teeth.

Tooth powder:It is structurally oldest and simplest preparation and they are also the cheapest. It is the
dry powder.

Formulation:
1. Abrasives: Eg: Sodium meta phosphate
2. Surface active agents: Eg: Sodium lauryl sulphate.
3. Sweetening agents: Eg: Saccharin,Aspartate.
4. Flavouring agents: Eg: Peppermint oil

Tooth paste contains additional ingredients

 Binding agents: Eg: Corragenan, Gum Tragacanth.

 Humectants: Eg: Glycerol, Sorbitol
 Preservatives: Eg: Methylparaben.
 Therapeutic agents: Eg: Urea,Chlorhexidine
 Miscellaneous agent: Eg: Titanium dioxide

Dental foams:
They are pressurized aerosol containers producing products. They had limited success. They are
pressurized with nitrogen.

Reference: Cosmetic technology by Sanju Nanda and Arun Nanda, Page no: 443-458.

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Observations and calculation

Specimen label

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Experiment No: 38
Date:
TOOTH PASTE

Aim: To prepare and submit 30g of tooth paste.

Formula:
Calcium carbonate 39.5%
Glycerine 15%
Tragacanth powder 0.4%
Sodium lauryl sulphate 6.3%
Saccharin sodium 0.1%
Peppermint oil 1.2%
Methyl paraben 0.5%
Water 32%

Principle:Toothpaste is the semisolid preparations with high percentage of solid particle. They are
meant to clean the surface of the teeth with the help of a tooth brush. Calcium carbonate used as
abrasives. Sodium lauryl sulphate used as surface active agent. Saccarin sodium is use as sweetening
agent. Glycerin used as humectent. Tragacant is used as binding agent.

Procedure:First dispersetragacanth powder in appropriate quantity of water and then addglycerine.

Addpowdered calcium carbonate, saccharin sodium and methyl parabengradually into the aqueous
mucilage with slowcontinuous stirring. After addition of all powders, add peppermint oil.Add sodium
lauryl sulphateat the end. Stir well avoiding vigorous agitation.

Use: As a dentifrice in cleaning teeth

Report :

Reference: Cosmetic technology by Sanju Nanda and Arun Nanda, Page no: 447.

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Observations and calculation

Specimen label

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Experiment No: 39
Date:
TOOTH POWDER

Aim:To prepare and submit 10 g of tooth powder.

Formula:
Calcium carbonate 76g
Kaolin 21g
Sodium lauryl sulphate 2g
Saccharin sodium 0.1g
Flavour qs

Principle: It is a cleanser consisting of abrasives, flavouring agents and sweetening agents in fine
powder form. Calcium carbonate used as abrasives. Sodium lauryl sulphate used as surface active agent.
Saccharine sodium used as sweetening agent. Peppermint used as flavouring agent.

Procedure:Separately weigh ingredients and triturate in a mortar and pestle. Pack in a wide mouthed
container.

Use: tooth cleansing agent

Report :

Reference: Cosmetic technology by Sanju Nanda and Arun Nanda, Page no: 446.

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Observations and calculation

Specimen label

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Experiment No: 40
Date:
ALKALINE SALINE MOUTHWASH

Aim:To prepare and submit 25 ml of alkaline saline mouthwash.

Formula:

Sodium chloride -8g

Sodium carbonate -4g
Amaranth solution -5ml
Peppermint water -qs
Principle: A mouth wash is an aqueous solution which is used for its deodorant, refreshing and an
antiseptic effect in the oral cavity .Water is the simplest mouth wash and the aqueous saline is the least
complex mouth wash. They are used as therapeutic aids in the treatment of mucosal diseases. Here
Peppermint water is used as the flavouring agent.Sodium chloride used to make the solution isotonic.
Sodium carbonate is used to dissolve the mucous and washes the throat, which is added to spray
solutions.Amaranth solution is used as colouring agent.

Procedure: Mix required amount of sodium chloride and sodium carbonate and dissolve in peppermint
water. Add amaranth solution and make up the volume with peppermint oil.

Use:Deodorizing oral cavity.

Precaution: Do not swallow

Report :

Reference: Cosmetic technology by Sanju Nanda and Arun Nanda,Page no:462.

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 DEPILATORIES
It is used for degradation of superficial hair chemically without affecting the skin.Depilation means
removal of hair as a result of chemical degradation without affecting the skin. For example byinorganic
sulphide and organic thiols.Epilation means relatively intact hair is removed by uprooting, for example
by plucking electrolysis, X-ray or by topically applied thallium composition. In majority of the case
the hair should be softened swelled and disposed
Properties: It should be non toxic and non irritant.
It should be fast and efficient in its action.
It should be odourless
It should be easy to apply
It should be stable.
Mechanism of action:Hair containskeratin, the protein rich in sulphur containing amino acid
cysteine(17%). Cysteine is linked chemically with other non-sulphur aminoacid including aspartic acid
and glutamic acid. The deposition of the sulphur in the hair fibre becomes such as to form a s-s bridge
between polypeptide chains (R-CH2-S-S-CH2-R). Most of the chemical treatment involves the rupture
and reformation of s-s linkages. So hair will disintegrate.
For example alkalimetal sulphides,sulphites,cyanides,amines, mercaptans etc., the s-s bond in keratin
are affected.Increasing osmotic pressure develops within the hair fibre, which swells and loses its
tensile strength and generally deteriorates, a mass of jelly like consistency which can be easily removed.
Formulation:
Inorganic Sulphides :Eg:Sodium sulphide, Bariumsulphide.
Substituted mercaptans : Eg: Thioglycolates
Enzymes :Eg:Keratinase enzyme
Stannites : Eg:Sodium stannite

Other additives
Humectants : Eg: Glycerin, Sorbitol
Thickening Agent :Eg:Methyl cellulose, Starch
Accelerators : Eg: ureas,Thioureas
Hair growth retardants :Eg: herbal extracts.

Reference:Cosmetic technology by Sanju Nanda, Arun Nanda, Page no: 412.

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Observations and calculation

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Experiment No: 41
Date:
DEPILATORIES

Aim: To prepare and submit 10 g depilatory.

Formula: Barium sulphide - 8%

Calcium carbonate - 35%

Sodium lauryl sulphate - 1%

Glycerin - 2%

Water -54%

Principle:Depilation means removal of hair as a result of chemical degradation without affecting the
skin.In majority of the case the hair should be softened swelled and disposed. Barium sulphate helps in
the degradation of the hair particle by breaking the cystein bridges between the polypeptide chains.
Calcium carbonate is used to adjust pH of the formulation. Glycerin is used as humectants.Here sodium
lauryl sulphate used as emulsifiers.

Procedure: Accurately weigh Barium Sulphide, Calcium Carbonate, Sodium lauryl sulphate and then
finely powder using mortar and pestle. Add glycerin and sufficient quantity of water until a smooth
paste is obtained. Label and dispense the formulation.
Use: To remove unwanted hair.

Direction: For external use only

Report:

Reference:Cosmetic technology by Sanju Nanda and Arun Nanda, Page no: 412.

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 INTRODUCTION TO ACCELERATED STABILITY STUDIES

In the past it was a practice in many pharmaceutical industries to evaluate the stability of
pharmaceutical preparations by observing them for one year or more corresponding to the normal time
that they would remain in stock and in use. Such a method was time consuming and uneconomical. It
has therefore become essential to device a technique for finding out the stability of the product in a fast
rate. It is then possible to identify the most stable and suitable formulation. Predicting life of the product
may be made by accelerating the decomposition process and extrapolating the result to a normal
condition.

Acceleration of a chemical degradation is achieved by raising the temperature of preparation.

Application of the principle of kinetics to the result of accelerated storage test carried out at three or
more elevated temperature enables prediction to be made on the effective life of preparation at normal
temperature. The order of reaction for the decomposition process is determined by plotting the
appropriate function of concentration against time and obtaining a linear relationship. An Arrhenius
relationship k = Ae-Ea/RTis employed to determine the reaction velocity constant for the decomposition
at room temperature. The logarithm of the specific rate of decomposition is then plotted against
reciprocal of absolute temperatures and the resulting line is extrapolated to room temperature. The k25
is used to obtain a measure of the stability of the drug under ordinary shelf life conditions.

The quality below which a product is no longer acceptable will vary from product to product
depending upon the type of decomposition. For example, the level is often taken to be 90% of the initial
potency of the product. Alternatively it could be the level of which a toxic break down of the product
can no longer be tolerated or at which a certain degree of order or colour change in drug.

The Shelf Life:

It can be defined as the time during which the product will maintain the required quality (up to
90%). The shelf life of the elevated temperature is found out by plotting time versus log concentration
remained. The shelf life of room temperature is obtained from a linear plot of temperature 1/T taken
against log of days to remain 90 % concentration.

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There are mainly two methods for determination of shelf life by accelerated stability studies.

1. Garette and Carper method.

2. Free and Blythe method

Garette and Carper method

In this method the drugs are stored at elevated temperature ranging from 40-90°C. During
different time intervals, samples are withdrawn and the drug content is estimated. Then a graph is
plotted between concentration of drug versus time to obtain a straight line and slope of this graph permit
estimation of K value to one temperature. The K values at different temperatures are obtained in the
same way and log K values are plotted against reciprocal of absolute temperature (1/T).

Free and Blythe method

This is similar to Garette&Carper method but instead of concentration the log percentage of
drug remaining is plotted against time to yield a straight line. From this time to reach 90% for different
temperatures are found out and log time to 90% is plotted against 1/T. By extrapolating this graph to
room temperature, the time to reach 90% at room temperature can be found out. The degradation of
aspirin yield salicylic acid and acetic acid. Hence by finding concentration of aspirin at different
temperature, we can found out the concentration of aspirin remaining undecomposed and this can
accomplish by use of standard graph of salicylic acid. The shelf life of aspirin is then found out by
using the equation,

Shelf life = 0.014/K at 25ºC

Overage

The excess quantity of drug that must be added to the preparation is to maintain at least 100%
of the labeled amount during the expected shelf life of drug. This is also found out from the accelerated
stability studies.

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Limitation of Accelerated Stability Studies

(1) The predicted shelf life of a preparation will only be voted if the accelerated test is carried out in
the final packaging product.

(2) The accelerated testing technique can only be applied to those formulations in which the
decomposition is produced with increasing temperature.

(3) The shelf life prediction is only be applied to the product which is under investigation, cannot be
expected the prediction to be valid for different formulation of the same drug.

References: Physical pharmacy by Alfred martin, Page no: 392-394.

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Experiment No: 42
Date:

ACCELERATED STABILITY STUDIES

Aim:To determine the shelf life of aspirin solution in 0.1N HCl using accelerated stability study.

Requirements: 100mg salicylic acid, distilled water, 4% ferric nitrate, spectrophotometer, 100mg
aspirin, 0.1N HCl, standard flask, alcohol, thermometer.

Principle:In the past, stability of pharmaceutical preparations is evaluated by observing them for a year
or more, but such method was time consuming. Now accelerated stability study is carried out in many
companies, and accelerated stability study of chemical decomposition is achieved by raising the
temperature of the preparation. Accelerated stability studies are carried out by following steps:

(1) Acceleration of chemical decomposition is achieved by raising the temperature of preparation.

(2) Determine the order of the reaction whether it is zero order, first order or second order reaction.

(3) Determine the reaction rate constant at higher temperature.

(4) Plot log k versus 1/T the resulting line is extrapolated to room temperature and k for 250C is
obtained.

(5) From the k value we can determine the stability of the drug under ordinary shelf conditions.

Procedure:

Preparation of standard graph of salicylic acid:Weigh100mg of salicylic acid into a standard flask
and make upto 100ml with distilled water. Shakewell the contents to give concentration of 1mg/ml.
Prepare solutions of various concentration strength like 20,40,60,80 and 100 µg/ml by taking 1,2,3,4
and 5ml of stock solution and make upto 50ml. Take2ml each of the solution and add 2ml of 4% ferric
nitrate solution to develop colour. Note the absorbance at 547nm with a suitable colorimeter.

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Accelerated stability study of aspirin:Dissolve100mg of aspirin in 100ml of 0.1N HCl and addtwo
drops of alcohol for easy dissolution of the solute. Shakethe contents well and transferinto a conical
flask and incubate at 500C. Withdraw5ml of the sample from the conical flask and add2.5ml of 4%
ferric nitrate solution andobserve the absorbance at 547nm. Usea blank with 5ml 0.1N HCl and 2.5ml
ferric nitrate solution. Repeatthis procedure at 60 and 700C. Extrapolatethe corresponding
concentrations from the standard graph of salicylic acid and calculate log% of undecomposed aspirin.
Plot a graph with time on X-axis and log% of undecomposed aspirin on Y-axis. Find the K values for
all temperature by multiplying the slope by 2.303. Plot the graph with 1/T for different temperature X
axis and log k on Y axis, log k values at 250C can be extrapolated from the graph.

Shelf life = 0.014/K at 25ºC

Report:

References:Text Book of Physical Pharmacy, By Manavalan, Page no: 288

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 MICROENCAPSULATION

Microencapsulation is a process by which very tiny droplets or particles of liquid or solid material are
surrounded or coated with a continuous film of polymeric material.The product obtained by this process
is called as Microcapsules.Generally Micro particles consist of two components;
a) Core material.
b) Coat or wall or shell material

Core Material: The material to be coated. It may be liquid or solid or gas. Liquid core may be dissolved
or dispersed material.Core material contains drug, additive like diluents and stabilizers.

Coating Material: It is the inert substance which coats on core with desired thickness. Coating material
composed of inert polymer, plasticizer, coloring agent, resins and release rate enhancers or retardants.

Examples of Coating Materials

1. Water soluble resins- Gelatin, Gum Arabic, Starch, PVP, CMC, MC, Polyvinyl alcohol.
2. Water insoluble resins- EC, Polyethylene, Polymethacrylate, Polyamide (Nylon), Cellulose nitrate.
3. Enteric resins- Shellac, Cellulose acetate phthalate, Zein.

Advantages:
 To protect reactive substances from the environment.
 To separate incompatible components for functional reasons.
 To control release of the active components.
 To mask the unpleasant taste or odor of the drug.
 To increase of bioavailability and produce a targeted drug delivery.
 Protects the GIT from irritant effects of the drug.

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Methods for microencapsulation
 Air suspension
 Coacervation phase separation
 Multiorifice-centrifugal process
 Spray drying and congealing
 Pan coating
 Solvent evaporation techniques
 Polymerization

Reference:Controlled Drug Delivery - concepts and advances, S.P Vyas and R.K Khar, Page no: 174

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Observations and calculation

Ingredients Official formula Working formula

Sodium alginate 5% 5g

Calcium chloride 2% 2g

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Experiment No: 43
Date:
PREPARATION OF CALCIUM ALGINATE BEADS

Aim:To prepare and submit calcium alginate bead.

Principle:Microencapsulation method using here is known as cross linking method. Drug is

encapsulated by alginate as it forms the microsphere. Alginate is a material which is natural polymer
obtained from blue-green algae. It is composed of 2 unit glucuronic acid and mannuronic acid. They
have same structure as glucose. They will combine to form the polymer alginate which is availableas
sodium salt.
When this solution is added to calcium chloride solution, the alginate is replaced by calcium.
As calcium is divalent two chains will be attached to it and it gets converted to solid sphere. Upon
dying shrinkage occurs and fixedsize will be in micro meters, hence called microspheres. Calcium
alginate is a heat sensitive polymer.

Drug release can be controlled by

(1)Controlling the group in the matrix (formed by crosslinking of polymer).

(2) By increasing rigidity (Eg: Change in Ca2+ by Fe3+)

Procedure:Dissolvethe required amount of sodium alginate in 30 ml of water under gentle agitation to

givea concentration of 1% w/v. Extrude the resulting preparation drop wise through a needle into 100
ml of 1% calcium chloride solution at room temperature. The beads formed are allowed to remain in
stirred solution for 10minutes. Filterthe beads and wash withwater and dry at50ºC in an oven.

Report:

Reference:

Donald L.Wise; Handbook of Pharmaceutical Controlled release technology; page no: 329 – 343.

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