GSP Industrial Pharmacy-I Lab Manual

GITAM INSTITUTE OF PHARMACY
Name :
Reg. No. :
Class : B. Pharmacy Vth Semester
Subject Code & Name : BP 506P & INDUSTRIAL PHARMACY - I
(DEEMED TO BE UNIVERSITY)
(Estd. u/s 3 of the UGC Act 1956)
RUSHIKONDA, VISAKHAPATNAM
ANDHRA PRADESH - 530045
Website: www.gitam.edu
GITAM INSTITUTE OF PHARMACY
GANDHI INSTITUTE OF TECHNOLOGYAND MANAGEMENT
(Declared as Deemed to be University u/s 3 of UGC Act, 1956)
Accredited by NAAC with A+ Grade
Visakhapatnam Campus
Andhra Pradesh, India 530045
CERTIFICATE
Name: Class:
Roll No: Exam No:
Institution
This is certified to be the bonafide work of the student in the
Laboratory during the academic year 20 / 20
No. of practicals certified out of in the subject of
Teacher In –charge
Examiner’s Signature Principal
Date: Institution Rubber Stamp

Subject: Industrial Pharmacy-I Subject code: BP 506P
Instructor: Dr. Prasanthi Boddu and Dr. G. V. Radha
INDEX
Expt. Name of the Experiment
No.
Page No. Date of Signature
Experiment
1. Preformulation studies on
paracetamol
2. Preparation of paracetamol tablets by
wet granulation method
3. Evaluation of prepared paracetamol
tablets
4. Quality control test of marketed
Paracetamol tablets as per I.P
5. Preparation of aspirin film-coated
tablets
6. Evaluation of aspirin film-coated
tablets
7. Preparation and evaluation of
tetracycline hydrochloride capsules
8. Quality control test of marketed soft
gelatin capsules as per I.P
9. Preparation of ascorbic acid injection
10. Preparation of atropine sulphate eye

drops
11. Preparation of cold cream
Industrial Pharmacy – I Practical Manual
Experiment Number: 1 Date:
PREFORMULATION STUDIES ON PARACETAMOL

AIM: To determine preformulation parameters of the pure drug - paracetamol.
REQUIREMENTS: Bulk density apparatus, specific gravity bottle (pycnometer), measuring
cylinder, weighing balance, funnel, burette stand, graph paper, scale, clamp and paracetamol.
PRINCIPLE:
Preformulation commences when a newly synthesized drug shows sufficient pharmacological promise in animal
models to warrants evaluation in man. These studies should focus on properties of a new compound that could
effect the drug performance in development of efficacious dosage form. A thorough understanding of these
properties may ultimately provide a rationale for formulation design or support the need for molecular
modification.
DEFINITION: Preformulation involves the application of biopharmaceutical principles to physicochemical

parameters of drug substance are characterized with a goal of designing optimum drug delivery system.
Characterization of drug molecule is a very important step of preformulation stage of product development.
PROCEDURE FOR CONDUCTION OF PREFORMULATION STUDIES
LITERATURE/BACKGROUND OF THE DRUG

SUBSTANCE:
NAME OF THE COMPOUND: Paracetamol
STRUCTURE:
CHEMICAL NAME : 4-amino acetanilide

MOLECULAR WEIGHT : 151.2 g
MOLECULAR FORMULA : C₈H₉NO₂
THERAPEUTIC CATEGORY: Analgesic, antipyretic
SOLUBILITY : Freely soluble in 95% ethanol and acetone,
Sparingly soluble in water,
Very slightly soluble in ether and dichloro methane.
DOSE: 500 mg – 1 g every 6 hrs
STORAGE: Store protected from light and moisture
ORGANOLEPTIC CHARACTERISTICS:
4
COLOUR: White crystalline
GITAM Institute powder. Visakhapatnam
of Pharmacy,
SOLID STATE ANALYSIS/BULK CHARACTERIZATION:

PARTICLE SIZE DISTRIBUTION:
It is determined by sieving method. A known amount of sample was taken and placed on a set of sieves arranged
in descending order of their sieve size. The sieves along with the drug were placed on a sieve shaker and were
shaken for 15 minutes.
S.NO Sieve no: Mean size of Weight %weight Cumulative nd
(passed/retained) opening(µ) retained retained %weight
(d) (n) retained
1
2
3
4
Average particle size = ∑nd/∑n
Bulk density, true density and percentage porosity are the important derived properties of
powders. The knowledge of these properties is very important for the formulation of different
dosage forms in pharmacy.
BULK DENSITY: Apparent bulk density (ρb) was determined by placing the granules into a graduated cylinder
and measuring the volume (Vb) and weight (M) “as it is”.
The bulk volume includes the true volume, volume of inter-particle spaces and intra- particle pores. The packing
of particle mainly responsible for bulk. The particle may pack in such a way to have large gaps between their
surface are known to be as light powders or powders of low bulk density. If the gap between the particle surfaces
are small are called as heavy powders orpowders of high bulk density.
pb = M/Vb
Weight of sample =
Volume of sample =
Bulk density =
True density is the density of the material itself, excluding of the voids in the inter-
particular pores. It is defined as the ratio of mass of powder to its true value.
𝑊𝑒𝑖𝑔ℎ𝑡 𝑜𝑓 𝑡ℎ𝑒 𝑝𝑜𝑤𝑑𝑒𝑟 𝑔

𝑇𝑟𝑢𝑒 𝑑𝑒𝑛𝑠𝑖𝑡𝑦, 𝜌𝑝 = … … (2)
𝑇𝑟𝑢𝑒 𝑣𝑜𝑙𝑢𝑚𝑒 𝑜𝑓 𝑡ℎ𝑒 𝑝𝑜𝑤𝑑𝑒𝑟 𝑐𝑐 5
GITAM Institute of Pharmacy, Visakhapatnam
TAPPED DENSITY: The measuring cylinder containing a known mass of granules was tapped for 100 times
using a bulk density apparatus. The minimum volume (Vt) occupied in the cylinder and the weight (M) of the
granules was measured. The tapped density (pt) was calculated using the formula.
pb = M/Vb
Tapped volume =
Tapped density =
CARR’S CONSOLIDATION INDEX: It is the measure of potential strength that a power could build up in its
arch in a hopper and also the ease with which such an arch could be broken. Compressibility index of the granules
was determined by using the formula.
CI (%) = [(pt-pt/pt)] x 100
Carr’s index (%) Type of flow

5-15 Excellent
12-16 Good
18-21 Fair to passable
23-35 Poor
33-38 Very poor
>40 Extremely poor
Bulk density =
Tapped density =
CI =
HAUSENER’S RATIO: It is the measure of the flow property of the drug.

Hausener’s ratio = pt/pb
POROSITY is defined as the ratio of void volume to the bulk volume.

𝑉𝑜𝑖𝑑 𝑣𝑜𝑙𝑢𝑚𝑒
(𝑇𝑟𝑢𝑒 𝑑𝑒𝑛𝑠𝑖𝑡𝑦 – 𝐵𝑢𝑙𝑘 𝑑𝑒𝑛𝑠𝑖𝑡𝑦)
% 𝑝𝑜𝑟𝑜𝑠𝑖𝑡𝑦, ∈ = 𝑋 100
𝑇𝑟𝑢𝑒 𝑑𝑒𝑛𝑠𝑖𝑡𝑦
6
ANGLE OF REPOSE: It is the maximum angle possible between the surface of the pile of the powder and the
horizontal plane. The angle of repose was measured by using funnel method, which indicates the flow ability of
the granules. It is designated by θ. Angle of repose is determined by the following formula.
Tan θ = h/r
Where θ = angle of repose
h and r are the height and radius of the powder cone.
θ = Tan-1 h/r
θ=
The angle of repose and the flow properties of powder are provided in the table given below
Angle of repose (θ) Type of flow
<25 Excellent
25-30 Good
30-40 Fair/passable*
>40 Very poor
* Adding glidant, may improve flow
Lower the angle of repose, the better the flow properties. Higher the value of angle of repose,
the flow property is poor. The improper flow is due to frictional forces between the particles. These
are quantified by angle of repose. Angle of repose is expressed in degrees.
Paracetamol is used as antipyretic and the dose of the drug is high. The drug has poor
compressibility properties. Hence before it is prepared as tablets its preformulation studies need to
be assessed as it helps in choosing right excipients for tablet preparation.
PROCEDURE:
a. BULK DENSITY:
1. Weighed about 10 g of paracetamol powder and passed through the U.S standard sieve 20#.
2. The powder was filled in a 50 ml measuring cylinder and the initial volume was read from
the scale of the measuring cylinder in terms of ml.
3. Fixed the measuring cylinder on the table of bulk density apparatus.
4. Adjusted the knob for 100 tapings and the apparatus was started.
5. The volume of the powder at the end of the tapings was noted.
6. The apparatus was switched off when two subsequent values were same and the final and
constant reading was noted
7. After measuring the final volume as the bulk volume, the bulk density of drug was
calculated using the equation.
7
b. TRUE DENSITY
1. A clean and dried pycnometer or specific gravity bottle was taken and its weighed was
taken. The weight was noted as W1.
2. The empty bottle was filled with liquid (benzene) and weighed. The weight was noted as
W2.
3. Bottle was removed and washed with acetone and dried.
4. The bottle is now filled with given drug (about 2 g).
5. Now the liquid (benzene) was added slowly with gentle swirling.
6. Care should be taken to avoid the entrapment of air bubbles.
7. The weight of the bottle, powder and liquid before liquid displacement was taken as W3.
8. The weight of the bottle, powder and liquid after liquid displacement was taken asW4.
9. The difference in weight, i.e., W3-W4 is true volume of the powder.
10. Calculated true density as per the above-mentioned equation.
c. PERCENTAGE POROSITY
Percentage Porosity was calculated by substituting the values of bulk volume and true volume.
d. ANGLE OF REPOSE
1. A clean and dry glass funnel was fixed with a clamp to the iron stand.
2. Placed a glass plate on the table and arranged it below the glass funnel. a graph paper
was placed on the glass plate.
3. Weighed approximately 10 g of paracetamol drug.
4. Poured the drug into the funnel while blocking the orifice of the funnel by thumb.
5. Removed the thumb. The powder flows down onto the graph paper and formed a cone
shaped pile.
6. Now adjust the funnel clamp so that the gap between the bottom of the funnel and peak
of the powder pile at about 3 mm (2 - 4 mm).
7. Four points were marked (which are opposite) to each other on the circular base on the
graph paper, measure the diameter (d) and then radius (r).
8. The height of the pile was measured by keeping one of the rulers vertically and the
other horizontally to touch the peak of the pile. The reading of the vertical scale,
represents the height (h) of the pile.
9. Substituted the values in the above given equation and calculated the angle of repose.
REPORT:
8
PREPARATION OF PARACETAMOL TABLETS
AIM: To prepare and submit 10 Paracetamol tablets by wet granulation method.
REQUIREMENTS: Paracetamol, lactose, Starch, magnesium stearate, talc, water, beaker,measuring

cylinder, filter paper, mortar, spatula, glass rod, butter paper, sieves, punching machine.
General working formula:
S. No. Ingredients Qty per tablet) Qty required for 10

(mg) tablets
1 Paracetamol 500 5000
2 Starch paste (15%) q.s. q.s.
3 Lactose 50 500
4 Starch powder 30 300
5 Talc 2 20
6 Magnesium Stearate 1 10
Total weight of each tablet = 600 mg
THEORY AND PRINCIPLE: Tablets are unit solid dosage forms containing medicaments with
or without excipients which were compressed together using punches and dies. There are different
types of tablets. Tablets are the most convenient dosage forms taken by oral route. Conventional
tablets are simple tablet formulations from which the drug will release and reach the systemic
circulation with in a period of 30 minutes and will disintegrate in less than 10 minutes.
The advantages of tablets they provide elegant product identity, Free of defects like chips, cracks,
discoloration, and contamination, sufficient strength to withstand mechanical shock and agitation
during its production, packaging, shipping and dispensing good provide chemical stability and
physical stability.
9
The tablets may be made by wet granulation, dry granulation and direct compression methods. The
preliminary requirements for compression are a free flow of material from hopper into die cavity.
If the drug-excipient blend possesses good flow property, then it may be compressed without granulation
(direct compression) and the drug having higher dose/moisture/heat sensitive and not having the required
flow property, then it may be compressed by dry granulation and the widely employed technique is wet
granulation method. The size of the granule should be optimized as it may affect tablet weight, hardness,
friability and disintegration time.
Paracetamol is an antipyretic agent used in treatment of pyrexia as these tablets are conventional tablets the
disintegration time is around 10 minutes and the drug should reach systemic circulation within 30 to 45
minutes. Here the starch powder is taken as disintegrating agents (intragranular and intergranular), starch
paste acts as a binder. Lactose is used as diluent. Magnesium stearate is used as lubricnat and talc is used
as glidant.
PROCEDURE:
Preparation of starch paste:
1. The required quantity of starch was taken and dissolved in small volume of cold water.
2. The remaining water was taken in a beaker and heated on a water bath or hot plate.
3. Add the cold starch solution to the boiling water and till it form a viscous gel (translucent in color).
4. Cool the starch paste and use the same as a binder solution for preparing the granules.
Preparation of granules by wet granulation method:
1. Weighed quantity of Paracetamol, lactose andhalf quantity of starch was added in mortar and
mixed with pestle and blended well.
2. The binding agent (starch paste) was added slowly till the capillary stage (granule formation)
reaches.
3. The mass was then passed through the sieve no. 16.
4. Later they are dried in petri dish in a tray dryer at 45 to 50°C.
5. After drying the granules were passed through the sieve no. 22.
6. At this stage the remaining half amount of starch powder, magnesium stearate, talc (passed
through sieve no. 120) were added and mixed thoroughly.
7. The granules are weighed and percentage yield was calculated.
10
Tablet compression:
Finally, the granules (600 mg) were added in die cavities and compressed as tablets using rotary punching
machine.
PROCESSING SPECIFICATIONS:
Punch size: 13mm
Average weight per tablets: 600mg
Hardness: 4-5 kg/cm2
Thickness: 4 ± 0.2 mm
REPORT: Paracetamol tablets were prepared in 10 no. by wet granulation method and submitted.
11
EVALUATION OF PARACETAMOL TABLETS
AIM: To evaluate the prepared paracetamol tablets for various evaluation test.
REQUIREMENTS: Paracetamol tablets, tablet hardness tester, friability apparatus,

disintegration apparatus, water, beaker, measuring cylinder, filter paper.
THEORY AND PRINCIPLE: Quality control test ensure that the dosage form is stable, safe and
effective throughout its shelf life. Various official and unofficial evaluation test are there for tablets
The various official test for tablets are Dissolution, Content uniformity. Weight variation,
Disintegration and unofficial test are Mechanical strength, Tensile strength, Friability Test for
Tablets, Tablet size and shape, Thickness and Average weight. Hardness of a tablet can be
measured by the devices like Monsanto tester, strong-cobb tester, Pfizer tester, Erweka tester, key
tester etc.
Paracetamol is an analgesic and anti-pyretic drug which is poorly soluble in water. Paracetamol
dispersible tablets are prepared by wet granulation method. The prepared formulations were
passed the evaluation test i.e., weight variation, hardness and friability, percent drug content,
content uniformity, disintegration and dissolution studies.
Friability: Not more than 1%
Disintegration time: NMT 10 m
% drug content: 100 ± 5%
Dissolution test: in 900 ml of 0.1N HCl or 5.8 pH phosphate buffer at 37± 0.5° C at 100 rpm and
after dissolution as per standard procedure the in vitro drug release was calculated.
EVALUATION PROCEDURE
The formulate tablets were evaluated for the following physicochemical characteristics.
1. General appearance :
The formulated tablets were assessed for its general appearance.
A white round shaped tablet with a smooth appearance weighing about 600 mg each for formulated tablet.
Thickness
1. Thickness of the tablet is important to maintain uniformity of tablets weight.
12
2. The thickness of the tablets was tested for 3 tablets using calibrated vernier-calipers.
3. The tablets thickness was controlled with in a ± 5% variation.
Hardness:
1. Tablet was placed between two anvils of the hardness tester and applied the force to anvils
2. When the tablet breaks measured the reading and noted as the hardness of the tablet.
3. Repeated the test procedure with 2 tablets and calculate the average hardness (kg/cm2).
4. The tablet crushing strength that just causes the tablet to break is recorded
Weight Variation:
1. Taken 10 tablets randomly and determined their collective weight and individual weights.
2. The average weight was calculated from the collective weight.
3. The test pass not more than 2 of the individual weights deviate from the average weight.
4. Percentage shown in the table and none deviated by more than twice the percentage limit as per USP.
Average weight of tablet (mg) USP Average weight of tablet (mg) USP % difference
130/less 80/less 10
From 130 to 324 mg From 80 to 250 mg 7.5
More than 325 mg More than 250 mg 5
% deviation= (Each tablet weight-average weight)/Average weight * 100
S.No Weight of the Tablet % deviation (150mg-7.5%)

1
2
3
4
5
6
7
8
9
10
Friability:
1. Tablets corresponding to about 6.5 gm (if the average weight of tablet is equal to 650 mg
or less) i.e., approximately 10 tablets in case of tablets with average weight exceeding
650 mg.
13
2. Placed the tablets in the friability drum and rotated the drug 100 revolutions.
3. Drug rotation the tabletswere tumbled at a distance of 6 inches for each turn of the drum.
After 100 rotations the tablets removed and dedusted.
4. The weight of the tablets after dedusting was noted and the % friability was calculated from
the below mentioned equation. The value should not more than (NMT) 1.0%
% FRIABILITY =
Disintegration test:
1. The apparatus was cleaned as per the standard operating procedure.

2. The Basket-rack assembly was suspended in 1000 ml beaker containing distilled water.
3. The temperature was maintained at 37± 2°C.
4. Six tablets were transferred to each tube followed by addition of disc to each tube.
5. Operated the apparatus for 15 minutes in case of uncoated 30 minutes for film coated
and 60minutes for coated tablets other than film coated tablets.
6. Noted time taken for each tablet to completely disintegrate.
7. If any of the tablets fail to disintegrate then the test was repeated with additional 6 tablets
byomitting the discs in case of uncoated and coated tablets other than film coated tablets.
8. The tablets pass the disintegration test if all six tablets have disintegrated.
REPORT:
14
QUALITY CONTROL TEST OF MARKETED TABLETS AND CAPSULES AS PER I.P
AIM: To evaluate the marketed tablets of paracetamol as per I.P
REQUIREMENTS: Marketed tablets, tablet hardness tester, friability apparatus, disintegration

apparatus, water, beaker, measuring cylinder, filter paper.
The various official test are Dissolution, Content uniformity. Weight variation, Disintegration and
unofficial test are Mechanical strength, Tensile strength, Friability Test for Tablets, Tablet size and
shape, Thickness and Average weight. Hardness of a tablet can be measured by the devices like Monsanto
tester, strong-cobb tester, Pfizer tester, Erweka tester, key tester etc.
QUALITY CONTROL TESTS FOR TABLETS

Weight Variation:
3. The test pass not more than 2 of the individual weights deviate from the average weight
4. Percentage shown in the table and none deviated by more than twice the percentage.
Hardness:
3. Repeated the test procedure with 10 tablets.
15
Friability:
less) i.e approximately 10 tablets in case of tablets with average weight exceeding 650 mg.
Initial weight − final weight
%Friability = X 100
Initial weight

5. Operated the apparatus for 15 minutes in case of uncoated 30 minutes for film coated and 60
minutes for coated tablets other than film coated tablets.
7. If any of the tablets fail to disintegrate then the test was repeated with additional 6 tablets by
omitting the discs in case of uncoated and coated tablets other than film coated tablets.
In vitro dissolution studies
1. The USP paddle method was used for in vitro dissolution studies of tablets.
2. Dissolution studies were performed in 900 ml of suitable dissolution medium.
3. Which is maintained at 37±0.5 ºC.
4. The rate of stirring was 50 rpm.
5. At appropriate intervals (5, 10, 15, 30, 45, 60 and 90 min), 5 ml of samples were taken and
filtered through 0.45 micron filter paper.
6. The samples were analysed at suitable wavelength using UV-visible spectrophotometer.
REPORT:
16
PREPARATION OF FILM-COATED ASPIRIN TABLETS
AIM: To prepare and evaluate directly compressible film-coated tablets of Aspirin.
REQUIREMENTS: Aspirin, lactose, microcrystalline cellulose, starch, magnesium
stearate
THEORY:
Tablets are the most common solid oral dosage form for many reasons including ease of
manufacturing, convenience for the patient, accurate dose administration, and better stability
than liquids and parenteral dosage forms.
Direct compression is the simplest and most economical method for the manufacturing of
tablets because it requires less processing steps than other techniques such as wet granulation
and roller compaction.
The manufacturer can blend an API with the excipients and the lubricant, followed by
compression, which makes the product easy to process. No additional processing steps are
required. Moisture or heat sensitive ingredients, which would be contraindicated in wet
granulation, can also be used in this type of process.
Aspirin is used as a analgesic and pain killer. Since the drug has good compressibility ability
it was directly compressed as tablets without using wet granulation method. Lactose is used as
a diluent, MCC is added as a disintegrant, starch and talc were added as binder, disintegrating
agent and also to improve the flow properties of powders.
COMPOSITION OF FORMULATION (PER TABLET):
Ingredients F1 (weights in mg) Purpose

Aspirin 200 API
Lactose 152 Diluent
MCC 120 Disintegrants
Starch 20 Binder
Magnesium stearate 4 Lubricant
Talc 4 Glidant
17
FORMULATION: Aspirin tablets were prepared by direct compression
PROCEDURE:
1. Screened all powder ingredient of the mixture to remove any lumps or aggregates (with
sieve no. 22).
2. Weighed each ingredient according to the corresponding batch size of the formulation.
3. Blended the pre-weighed powder to make a homogenous powder mixture.
4. After proper mixing, the blend was placed in the hopper and weight adjustment was done.
The blend was compressed as tablets using punching machine.
PRINCIPLE:
A film is a thin polymer based coat applied to solid dosage form such as a tablets or granules. The
thickness of such a coating is usually between 20 – 100 microns. Tablets are passes through
spraying zone, where the adherent material is sprayed and allowed to dry. Film coating is generally
performed in two ways aqueous and non-aqueous film coating. Film coating has been applied to
improve stability and ease of ingestion without altering drug release characteristics.
Sr. No. Ingredients Quantity in %
1 Hydroxy propyl methyl cellulose 4g
2 Propylene glycol 1.2 mL
3 Ethyl alcohol 45 mL
4 Methylene Chloride q.s.
5 Titanium dioxide 0.5 g
6 Ferric oxide 1g
PROCEDURE:
Preparation of aqueous film coating solution:
1. The weighed quantity of ethyl alcohol and methylene chloride were taken in a beaker.
2. The film former, HPMC was added and stir it with a glass rod.
3. Plasticizer, propylene glycol was added to the beaker and mixed properly.
4. Titanium dioxide and ferric oxide colours were uniformly suspended in the polymer
dispersion.
5. The polymer dispersion was mixed thoroughly with constant stirring.
Coating process:
1. The aspirin tablets was coated with polymer dispersion film by dipping for 1 minute.
2. The tablets were allowed to dry in an oven for 15 minutes at 60 °C and usual atmospheric
pressure to obtain a pre coat.
REPORT: Aspirin film-coated tablets were prepared, dried and submitted.
18

EVALUATION OF ASPIRIN FILM COATED TABLETS
AIM: To perform film coating of tablets/granules
REQUIREMNTS: Tablet coating pan, hydroxyl propyl methyl cellulose, poly vinyl pyrolidone,
PEG 6000, PEG 200, titanium dioxide, sunset yellow, methyl paraben, propyl paraben.
PRINCIPLE: Quality control test ensures that the dosage forms is stable, safe and effective
throughout is shelf-life. Various official and non-official tests are there for tablets.
EVALUATION PROCEDURE
Thickness
1. Thickness of the tablet is important to maintain uniformity of tablets weight.

2. The thickness of the tablets was tested for 10 tablets using calibrated vernier-calipers.
3. The tablets thickness was controlled with in a ± 5% variation.
Hardness:
3. Repeated the test procedure with 10 tablets.
Weight Variation:
3. The test pass not more than 2 of the individual weights deviate from the average weight
4. Percentage shown in the table and none deviated by more than twice the percentage.
Average weight Percentage deviation
80 mg or less 10
More than 80 but less than 250 mg 7.5
250 or more 5
19
Friability:
or less), approximately 10 tablets in case of tablets with average weight exceeding 650 mg.
Initial weight − final weight

%Friability = X 100
Initial weight

5. Operated the apparatus for 15 minutes in case of uncoated 30 minutes for film coated and 60
minutes for coated tablets other than film coated tablets.
7. If any of the tablets fail to disintegrate then the test was repeated with additional 6 tablets by
omitting the discs in case of uncoated and coated tablets other than film coated tablets.
REPORT:
20
PREPARATION AND EVALUATION OF TETRACYCLINE HYDROCHLORIDE

CAPSULES
AIM: To prepare and evaluate tetracycline hydrochloride capsules.
REQUIREMENTS: Tetracycline hydrochloride, dried starch, dried talc, capsule (1 size),

mesh, mortar, and pestle, stirrer, capsule filling machine, beaker, glass rod, measuring cylinder,
funneland electronic digital balance.
CATEGORY: Board spectrum antibiotic
USUAL STRENGTH: 250 mg, 500 mg
FORMULA:
Sr. No. Name of the ingredient Quantity for 1 Quantity for 10 capsules
capsule
1 Tetracycline hydrochloride 250 mg 2500 mg
2 Dried starch 25 mg 250 mg
3 Dried talc 25 mg 250 mg
Total weight 300 mg
PRINCIPLE: Capsules are unit solid dosage forms where the active pharmaceutical ingredient is
filled and enclosed in an empty hard gelatin capsule. Capsules provide a tasteless and color less
dosage form without the need for a secondary coat. The unpleasant drugs can be formulated as
capsules for taste masking as the empty capsules shell are tasteless. The maximum fillable
capacity of the powder in “1” size capsule is 400 mg. Tetracycline hydrochloride is used as an
antibiotic, dried starch is a diluent added to adjust the weight, and talc is a glidant.
PREPARATION OF TETRACYCLINE HYDROCHLORIDE CAPSULES
1. Clean all the equipment’s as per the standard operating procedure.

2. Pass the drug through 60# mesh sieve into a blender.
3. In a separate container pass and collect dried starch and talc through 80# mesh sieve.
4. Add the above ingredients into drug and blend it for 10 minutes.
21
5. Fill the prepared blend into the empty capsules body using suitable capsule filing
equipment.
EVALUATION PARAMETERS
PREFORMATION STUDIES OF POWDER/GRANULES
Angle of repose:
1. The angle of repose was measured according to the fixed funnel and cone method.
2. The powders were allowed to flow through the funnel until a conical pile is formed.
3. The angle of repose was determined as follows:
h
tan θ =
r
Where, θ is the angle of repose, h is the height of heap and r is calculated from the mean diameter
of the powder cone.
Relationship between angle of repose and powder flow properties
Angle of repose (º) Powder flow properties

<25 Excellent
25-30 Good
30-40 Fair
41-45 Passable
46-55 poor
56-65 Very poor
>65 Very very poor
Bulk density:
1. The weighed quantity of powder systems were placed in a graduated cylinder and the
volume occupied (bulk volume 𝑉𝑏) and weight (M) were recorded.
M
Bulk density (ρbulk ) =
Vb
22
Tapped density: The weighed quantity of graduating cylinder was tapped for several times till a
constant volume was obtained and the volume of powder (tapped volume 𝑉𝑡) and weight (M) were
recorded.
M
Tapped density (ρ tap ) =
Vt
Bulk and tapped densities used to calculate the Carr’s index and Hausner’s ratio
Carr’s index (CI%): Carr’s index was obtained from the bulk and tapped densities by the
following equation:
ρtap − ρbulk
Carr′s index =
ρtap
Where, 𝜌𝑏𝑢𝑙𝑘 is the freely settled bulk density of the powder and 𝜌𝑡𝑎𝑝is the tapped bulk density of
the powder.
The smaller the value of the CI%, the superior the flow properties of the powder.
Hausner’s ratio (HR): Hausner ratio was calculated according to the following equation:
𝜌𝑏𝑢𝑙𝑘
Hausner ratio =
𝜌𝑡𝑎𝑝
A high HR value means poor flow
Ranges of CI, HR and flow character
CI (%) HR Flow character

≤ 10 1.00-1.11 Excellent
11-15 1.12-1.18 Good
16-20 1.19-1.25 Fair
21-25 1.26-1.34 Passable
26-31 1.35-1.45 Poor
32-37 1.46-1.59 Very poor
> 38 > 1.60 Very very poor
23
EVALUATION OF HARD GELATIN CAPSULE
Weight variation
1. 10 capsules from each batch selected at random and take the individual and average
weight.
2. The capsule pass the test if the weight of individual capsules falls within 90-110%
ofaverage weight.
Moisture content
1. According to USP the unit dose container is packed along with dehydrated pellets.
2. The weight of the test capsule compared with under test capsule.
3. The difference in weight gives the amount of moisture absorbed.

4. Six capsules were transferred to each tube followed by addition of disc to each tube.
5. Operated the apparatus for 30 minutes.
6. Noted time taken for each capsule to completely disintegrate.
REPORT:
24

QUALITY CONTROL TESTS FOR MARKETED SOFT GELATIN CAPSULE
AIM: To evaluate the marketed soft gelatin capsules as per I.P
REQUIREMENTS: Marketed capsules, disintegration apparatus, water, beaker, measuring

cylinder, filter paper.
The various official test are Dissolution, Content uniformity, Weight variation, Disintegration and
unofficial test are Mechanical strength, Tensile strength, Capsule size and shape, locking length and
Average weight.
QUALITY CONTROL TESTS FOR TABLETS
Weight variation
1. 20 capsules from each batch selected at random and take the individual and average
weight.
2. The capsule pass the test if the weight of individual capsules falls within 90-110% of
average weight.
Moisture content
1. According to USP the unit dose container is packed along with dehydrated pellets.
2. The weight of the test capsule compared with under test capsule.
3. The difference in weight gives the amount of moisture absorbed.

4. Six capsules were transferred to each tube followed by addition of disc to each tube.
5. Operated the apparatus for 30 minutes.
6. Noted time taken for each capsule to completely disintegrate.
REPORT:
25
Experiment Number: 9 Date
PREPARATION OF ASCORBIC ACID INJECTION
AIM: To prepare and evaluate 10 ml of ascorbic acid injection
REQUIREMENTS: Ampoules, beaker, measuring cylinder, membrane filter, pH meter
CHEMICALS: Ascorbic acid, disodium edetate, sodium hydroxide, sodium bicarbonate, water
for injection.
THEROY AND PRINCIPLE:
Sterile products are dosage forms of therapeutic use that are free from viable microbes. Parenteral
should be free from toxic components as well as possess an exceptionally high level of purity. The
formulation of parental products involves combination of one or more ingredients with a medicinal
agent enhance the convenience and acceptability of product.
FORMULA:
S. No. Name of the ingredients Quality for one Quantity for 5

ampoule ampoules
1 Ascorbic acid 2.5 g
2 Disodium edentate 2.5 mg
3 Sodium hydroxide 1.1 g
4 Sodium bicarbonate 1.45 g
5 Water for injection q.s. 10 ml
PROCEDURE:
Procedure for preparation of water for injection
1. Distilled portable water from a neutral glass or metal still fitted with an efficient device
from preventing the entrapment of droplets.
2. Reject the first portion of distillate.
3. Collect remaining amount of water in suitable container.
4. Immediately sterilize by autoclaving or by filtration without addition of a bacteriostatic.
26
Procedure for preparation of ascorbic acid injection:
1. Type I glass ampoules are selected and clean. The formulation is carried out in clean area.
2. Weigh accurately about 2.5 gm of ascorbic acid and dissolved in 2/3rd of total volume of
water for injection.
3. Add sodium bicarbonate slowly with continuous stirring, effervescence will produce
4. Add disodium edentate and sodium hydroxide and stir to dissolve
5. Makeup the volume of preparation with help of remaining water for injection
6. Adjust the pH in between 5.5 - 6.5
7. Sterile the solution by passing through 0.22 µm membrane filter and fill the ampoule with
syringe and seal.
REPORT: Ascorbic acid injection was prepared, sealed, sterilized and submitted.
27
PREPARATION OF ATROPINE SULPHATE EYE DROPS

AIM: To prepare and submit 30 ml of atropine sulphate eye drops.
REQUIREMENTS:
Atropine sulphate, sodium chloride, sterile purified water, autoclave, membrane filter etc.
GENERAL FORMULA:
Atropine sulphate 300 mg
Sodium chloride 234 mg
Sterile purified water 30 ml
PRINCIPLE:
Eye drops are sterile aqueous or oily solutions or suspensions of drugs that are instilled
into the eye with a dropper. They are used for both diagnostic and therapeutic purposes.
They usually contain the drugs used as antimicrobial agents, anti-inflammatory agents,
diagnostic stains, corticosteroids and artificial tears. They also contain the drugs used in the
treatment of glaucoma, local ananesthetics, miotic and mydriatics.
PROCEDURE:
1. Weigh and measure all the required ingredients of eye drop properly and keep them
separately.
2. Take 50 ml beaker and dissolve sodium chloride in sterile purified water.
3. Add atropine sulphate and dissolve it by continuous shaking.
4. The eye drop is clarified by passing through membrane filter.
5. Sterilize the product by autoclaving at 121 °C for 30 minutes.
LABEL: For external use only and store in a cool and dry place.
STORAGE: Store in a cool & dry place.
CATEGORY: Dilates the pupil of the eye.

REPORT:
28
PREPARATION OF COLD CREAM

AIM: To prepare and submit 10 g of cold cream.
REQUIREMENTS:
White bees wax, Liquid paraffin, Borax, Purified water, etc.
GENERAL FORMULA:
White bees wax 10 g
Liquid paraffin 6g
Borax 0.1 g
Purified water 1.9 g
PRINCIPLE:
Creams are viscous semi-solid emulsions which are meant for external applications.
Creams contain a water soluble base due to which they can be easily removed from the skin. They
are of softer consistency and have light in weight in comparison to ointment when applied on to
the skin. Creams leave no visible evidence of their presence on the skin.
Cold cream is an oily cream. It is w/o type of emulsion. These creams are greasy.
PROCEDURE:
1. Melt the white bees wax on a water bath by the application of heat.
2. Then add liquid paraffin and raise the temperature of the mixture to 70 oC.
3. Dissolve borax in purified water and heat the solution to 70 oC.
4. Gradually add the boric acid solution to the melted mixture and until cool to room
temperature.
5. Then transfer to a well closed container, label and dispense.
LABEL: For external use only.
CATEGORY: Emollient and protective.
STORAGE: Stored in a cool place.
REPORT: Cold cream was prepared and submitted.
29

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GITAM INSTITUTE OF PHARMACY

Class : B. Pharmacy Vth Semester

Subject Code & Name : BP 506P & INDUSTRIAL PHARMACY - I

Roll No: Exam No:

This is certified to be the bonafide work of the student in the

Laboratory during the academic year 20 / 20

No. of practicals certified out of in the subject of

Examiner’s Signature Principal

Date: Institution Rubber Stamp

10. Preparation of atropine sulphate eye

Experiment Number: 1 Date:

PREFORMULATION STUDIES ON PARACETAMOL

DEFINITION: Preformulation involves the application of biopharmaceutical principles to physicochemical

PROCEDURE FOR CONDUCTION OF PREFORMULATION STUDIES

LITERATURE/BACKGROUND OF THE DRUG

CHEMICAL NAME : 4-amino acetanilide

SOLID STATE ANALYSIS/BULK CHARACTERIZATION:

Average particle size = ∑nd/∑n

𝑊𝑒𝑖𝑔ℎ𝑡 𝑜𝑓 𝑡ℎ𝑒 𝑝𝑜𝑤𝑑𝑒𝑟 𝑔

Carr’s index (%) Type of flow

HAUSENER’S RATIO: It is the measure of the flow property of the drug.

POROSITY is defined as the ratio of void volume to the bulk volume.

Experiment Number: 2 Date:

PREPARATION OF PARACETAMOL TABLETS

AIM: To prepare and submit 10 Paracetamol tablets by wet granulation method.

REQUIREMENTS: Paracetamol, lactose, Starch, magnesium stearate, talc, water, beaker,measuring

General working formula:

S. No. Ingredients Qty per tablet) Qty required for 10

2 Starch paste (15%) q.s. q.s.

4 Starch powder 30 300

Total weight of each tablet = 600 mg

Preparation of starch paste:

Preparation of granules by wet granulation method:

Punch size: 13mm

Average weight per tablets: 600mg

Hardness: 4-5 kg/cm2

Experiment Number: 3 Date:

EVALUATION OF PARACETAMOL TABLETS

REQUIREMENTS: Paracetamol tablets, tablet hardness tester, friability apparatus,

Disintegration time: NMT 10 m

% drug content: 100 ± 5%

% deviation= (Each tablet weight-average weight)/Average weight * 100

S.No Weight of the Tablet % deviation (150mg-7.5%)

1. The apparatus was cleaned as per the standard operating procedure.

Experiment Number: 4 Date:

QUALITY CONTROL TEST OF MARKETED TABLETS AND CAPSULES AS PER I.P

AIM: To evaluate the marketed tablets of paracetamol as per I.P

REQUIREMENTS: Marketed tablets, tablet hardness tester, friability apparatus, disintegration

QUALITY CONTROL TESTS FOR TABLETS

1. The apparatus was cleaned as per the standard operating procedure.

In vitro dissolution studies

Experiment Number: 5 Date:

PREPARATION OF FILM-COATED ASPIRIN TABLETS

AIM: To prepare and evaluate directly compressible film-coated tablets of Aspirin.

REQUIREMENTS: Aspirin, lactose, microcrystalline cellulose, starch, magnesium

Ingredients F1 (weights in mg) Purpose

Lactose 152 Diluent

MCC 120 Disintegrants

Magnesium stearate 4 Lubricant

FORMULATION: Aspirin tablets were prepared by direct compression

3. Blended the pre-weighed powder to make a homogenous powder mixture.

Preparation of aqueous film coating solution:

REPORT: Aspirin film-coated tablets were prepared, dried and submitted.

Experiment Number: 6 Date: