Apt lab manual

GITAM INSTITUTE OF PHARMACY Page 1
PRACTICAL RECORD
INDUSTRIAL PHARMACY – I
B.Pharm V Semester
Prepared by
Dr.B.Prasanthi
M.Pharm., Ph.D., CSIR-RA
Assistant Professor
Department of Pharmaceutics
GITAM Institute of Pharmacy (GIP)
GITAM (deemed to be University)
Rushikonda, Visakhapatnam- 530045

Exp no: 1
Date:
PREFORMULATION STUDIES OF METRONIDAZOLE
AIM: To evaluate the preformulation parameters of metronidazole which include literature or back
ground of the drug substance, organoleptic characters, solid state analysis/bulk characterization,
solubility analysis, stability analysis and drug-excipient compatibility studies.
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.
DEFNITION: 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 : Metronidazole
 CHEMICAL NAME: 2-(2-methyl-5-nitro-1H-imidazol-1-yl) ethanol.
 MOLECULAR FORMULA: C6H9N3O3
 MOLECULAR WEIGHT: 171.2
MOLECULAR STRCTURE
 DESCRIPTION: White or yellowish crystalline powder.
 CATEGORY: Antiamoebic.
 DOSE: 200-400 mg.
 STORAGE: Store protected from light and moisture
 ORGANOLEPTIC CHARACTERISTICS:
COLOUR: White crystals or white crystalline powder.

SOLID STATE ANALYSIS/BULK CHARACTERIZATION:
PARTICLE SIZE ANALYSIS:
Microscopic method is the simplest technique in estimating the size ranges and shapes. A small
amount of the drug is taken and evenly spread on a glass slide. The eye piece was calibrated and the
particle size range was determined.
Calibration of micrometer:
1 division of stage micrometer = 0.01mm
N1 division of eye piece = N2 division of stage micrometer
…division of eyepiece = …division of stage micrometer
Least count of eyepiece = (N2/N1) x 0.1mm
S.NO Size range Mean size range x least
count(d)(µ)
Frequency (n) Nd
1
2
3
4
5
6
7
Arithmetic mean diameter = ∑nd/∑n
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:
(passed/retained)
Mean size of
opening(µ)
(d)
Weight
retained
(n)
%weight
retained
Cumulative
%weight
retained
nd
1
2
3
4
Average particle size = ∑nd/∑n

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”.
pb = M/Vb
Weight of sample =
Volume of sample =
Bulk density =
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

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.
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 =
Angle of repose (θ) Type of flow
<25 Excellent
25-30 Good
30-40 Fair/passable
>40 Very poor
SOLUBILITY ANALYSIS: The solubility of drug is an important physicochemical property
because it effects the bioavailability of the drug, the rate of drug release into dissolution medium and
consequently, the therapeutic efficiency of the pharmaceutical product.
The solubility of the molecules in various solvents is determined as a first step. This is a valuable
step in developing a formulation. Solubility is usually determined in variety of commonly used
solvents and some oils if the molecules are lipophilic. The solubility of material is usually
determined by the saturated/ equilibrium solubility method, which employs a saturated solution of
the material, where excess quantity of drug is taken in 10ml of each solvent and occasionally stirred
for 24hrs at room temperature and sample was filtered and filtrate was suitably diluted and analyzed
spectrophotometrically at 249nm.
Solubility Parts of solvent required for 1 part of solute
Very soluble Less than 1
Freely soluble From 1 to 10
Soluble From 10 to 30
Sparingly soluble From 30 to 100
Slightly soluble From 100 to 1000
Very slightly soluble From 1000 to 10000
Practically insoluble 10000 or more
The solvents used are distilled water, ethanol, chloroform and 0.1N HCl.

SOLUBILITY OF PARACETAMOL IN DIFFERENT SOLVENTS:
S.NO Solvent Absorbance Dilution
factor
Concentration
(mg/ml)
Solubility (parts required
to dissolve 1g of drug)
1. Water
2. Ethanol
3. 0.1 N HCl
4. Chloroform
pH: A 50% w/v drug solution was analyzed for its pH by using pH meter.
PARTITION COEFFICIENT: Partition coefficient (oil/water) is a measure of a drug’s
lipophilicity and an indication of its ability to cross cell membranes. It is defined as the ratio of
unionized drug distributed between the organic and aqueous phases at equilibrium.
10mg of drug was added to a mixture of 20ml of chloroform and 20ml of distilled water and it was
shaken for 30mins. After 30mins both phases are separated. Both phases were analyzed for amount
of drug by using UV-spectrophotometer.
Ko/w= concentration of drug in oil phase/ concentration of drug in aqueous phase.
Phase Absorbance Dilution factor Concentration
(mg/ml)
Aqueous layer
Organic layer
Ko/w =
CALIBRATION CURVE OF PARACETAMOL:
Concentration (µg/ml) Absorbance
0
2
4
6
8
10
STABILITY ANALYSIS:

SOLID STATE STABILITY:
ELEVATED TEMPERATURE STUDIES: The elevated temperature commonly used is 40, 50
and 60 oC with ambient humidity. The samples stored at highest temperature are observed for 2 to 3
hours in an open Petri dish for physical and chemical changes and compared to an appropriate
control. If a substantial change is seen, samples stored at lower temperature are examined. If no
change is seen at 60oC, the stability prognosis is excellent.
STABILITY UNDER HIGH HUMIDITY CONDITIONS: Solid drug samples can be exposed to
different relative humidity conditions by keeping them in laboratory desiccators containing saturated
solutions of various salts. The closed desiccators in turn are kept in oven to provide constant
temperature. The performulation data of this nature are useful in determining if the material should
be protected and stored in controlled low humidity environment or if non aqueous solvent be used
during formulation.
PHOTOLYTIC STABILITY: Many drugs fade or darken on exposure light. Though the extent of
degradation is small and limited to the exposed surface area, it presents anesthetic problem. The drug
sample was exposed to sunlight for 2 to 3 hours in an open Petri dish. Resulting data may be useful in
determining if an amber colored container is required or if color masking by should be used in the
formulation.
SOLUTION STATE STABILITY: As compared with the dry form, the degradation is much rapid
in solution form. It is important ascertain that the drug doesn’t degrade when exposed to GI fluid.
The pH based stability study, using different stimulator GI condition can be designed. A poor
solution stability of drug may urge the formulator to choose a less soluble salt form, provided the
bioavailability is not compromised.
a) Stability of drug in distilled water was determined by keeping known concentration of drug in
kinetic mode of UV-Visible spectrophotometer for 15mins with 90seconds interval.
Time ( seconds) Absorbance
0
90
180
270
360
450
540
630
720
810
900

b) Similarly stability of drug in 0.1N HCl was determined by keeping known concentration of
drug in kinetic mode of UV-visible spectrophotometer for 15mins with 90seconds interval.
Time ( seconds) Absorbance
0
90
180
270
360
450
540
630
720
810
900
DRUG EXCIPIENT COMPATIBILITY STUDIES: The knowledge of drug excipients
interactions is useful for the formulation to select appropriate excipients. The described
preformulation screening of drug excipients interaction requires only 5mg of drug in a 50% mixture
with the excipients to maximize the likelihood of obscuring an interaction.
a) A small amount of drug substance with one or more excipients in the ration of 1:1 are placed
in closed vials and placed at a temperature of 60 oC for a week. After storage the sample was
observed physically for liquefaction, caking, odour, gas formation and discoloration.
Drug + Excipient Observation
Drug alone
Drug + lactose
Drug + starch
Drug + crosscarmellose
Drug + magnesium stearate
Drug + talc
b) Determination of interference of additives in the estimation of drug:
The highest concentration of additives that could be present in 900ml of dilution beaker was
estimated on the basis of amount present for tablet of different batches with different additives were
taken in a 10ml volumetric flask. The flasks were kept for 24 hrs with occasional shaking and the
filtration was done. The filtrate was analyzed for drug concentration using UV-visible
spectrophotometer.

Optimized formula for solution stability studies:
Drug + excipient Quantity for 900 (mg) Quantity for 50 (mg)
Drug alone 500
Drug + lactose 500 + 100
Drug + starch 500 + 30
Drug + crosscarmellose 500 + 10
Drug + magnesium stearate 500 + 5
Drug + talc 500 + 5
Drug + excipient Absorbance Interference
Drug alone
Drug + lactose
Drug + starch
Drug + crosscarmellose
Drug + magnesium stearate
Drug + talc
REPORT:

Expt no: 2
Date:
FORMULATION AND EVALUATION OF METRONIDAZOLE
TABLETS AND COMPARISION WITH COMMERCIAL FILM
COATED METRONIDAZOLE TABLETS
AIM: To prepare and evaluate metronidazole film coated tablets.
APPARATUS: Dissolution apparatus, Disintegration apparatus, Friability apparatus, UV-Visible
spectrophotometer, Monsanto hardness tester.
CHEMICALS REQUIRED: Metronidazole, 0.1M hydrochloric acid, glacial acetic acid, 0.1N
perchloric acid, crystal violet.
DRUG PROFILE:
MOLECULAR STRUCTURE:
CHEMICAL NAME: 2-(2-methyl-5-nitro-1H-imidazol-1-yl) ethanol.
MOLECULAR FORMULA: C6H9N3O3
MOLECULAR WEIGHT: 171.2
DESCRIPTION: White or yellowish crystalline powder.
CATEGORY: Antiamoebic.
DOSE: 200-400 mg.
STORAGE: Store protected from light and moisture.
Formulation: 200mg dose tablets were formulated. 15 tablets were formulated by direct
compression.
Formulation table
S.no Ingredients Quantities (mg)/ each tablet
1 Metronidazole 200
2 Starch 30
3 MCC 65

4 Magnesium stearate 2
5 Talc 3
QUALITY CONTROL TESTS CONDUCTED:
HARDNESS: Hardness of tablets was determined by using Monsanto hardness tester. The lower
plunger was placed in contact with the tablets and a zero reading was taken. The plunger was then
forced against a spring by tuning a threaded bolt until the tablet fractured as the spring was
compressed a pointer rides along a gauge in the barrel to indicate the force.
FRIABILITY: The Roche friability test apparatus was used to determine the friability of the tablets,
20 pre-weighed tablets were placed in the apparatus which was given 100 revolutions. After which
the tablets were reweighed. The percentage friability was calculated.
Percentage friability = {(initial weight-final weight)/initial weight} × 100
DISINTEGRATION TEST: The disintegration test was carried out using the disintegration
apparatus which consist of a basket rack holding 6 plastic tubes, open at the top and bottom, the
bottom of the tube was covered by a 10-mesh screen. The basket was immersed in a bath of suitable
liquid held at 37ºC. 3 tablets were placed in tubes and time taken by tablet to disintegrate was noted.
DISSOLUTION:
 DISSOLUTION APPARATUS: Electro lab
 DISSOLUTION MEDIUM: 900ml of 0.1M hydrochloric acid.
 APPARATUS TYPE: USP2 {paddle type}
 SPEED: 100rpm
 SAMPLING: 5ml of sample was withdrawn at specified intervals of time (5, 10, 15,30,45,60
and 90 min) and at each time fresh solution was replaced. The obtained sample solutions
optical densities were measured at maximum at about 277nm against the blank using
spectrophotometer. The absorbance values were noted and compared with commercial film
coated tablets.
CALIBRATION CURVE OF METRONIDAZOLE:
CONCENTRATION (µg/ml) ABSORBANCE
0.0
2.0
4.0
6.0
8.0
10

FRIABILITY:
Formulated Tablet:
Initial weight of 10 tablets=
Final weight of 10 tablets=
%friability = (initial weight-final weight)/initial weight×100
=
Commercial Tablet:
Initial weight of 10 tablets=
Final weight of 10 tablets=
%friability = (initial weight-final weight)/initial weight×100
=
DISINTEGRATION TIME AND HARDNESS:
S.No Tablet DISINTEGARTION (in min) HARDNESS (kg/cm2)
1 Formulated
2 Formulated
3 Commercial
4 Commercial
DISSOLUTION TABLE FOR COMMERCIAL TABLET
S.No
Time
(min)
Absorbance
Concentration
(mg/ml)
%drug
release
%drug
unreleased
Log%drug
unreleased
1 0
2 5
3 10
4 15
5 20
6 30
DISSOLUTION TABLE FOR FORMULATED TABLET
S.No Time
(min)
Absorbance Concentration
(mg/ml)
%drug
release
%drug
unreleased
Log%drug
unreleased
1 0
2 5
3 10
4 15
5 20
6 30
7 45

8 60
9 90
10 120
TABLET
CORRELATION COEFFICIENT (r)
ZERO ORDER FIRST ORDER
FORMULATED
COMMERCIAL
REPORT:

Expt no: 3
Date:
EVALUATION OF ENTERIC COATED ASPIRIN TABLETS
AIM: To evaluate the enteric coated tablets of aspirin.
APPARATUS:
Dissolution apparatus, Disintegration apparatus, Friability apparatus, Monsanto hardness tester, U.V
spectrophotometer, compression machine.
CHEMICALS REQUIRED:
Salicylic acid, acetic anhydride, Sulphuric acid concentrated, 5% ferric chloride, 0.2M salicylic acid.
EVALUATION TESTS
IDENTIFICATION TEST:
Boil a quantity of the powdered tablets containing 0.3g of aspirin for 2 to 3 minutes with 10ml of 5M
sodium hydroxide, cool and add excess of 1M sulphuric acid, a crystalline precipitate is produced. To
this add iron (3) solution. Deep violet color is produced.
DISSOLUTION TEST:
In the apparatus 1000ml of 0.1M hydrochloric acid was filled and rotated the basket at 100
revolutions per minute. After 2 hours withdraw a sample of the medium, filter and measure the
absorbance of the filtrate at 276nm using 0.1MHCl in the reference cell. Measure the absorbance of a
suitable solution of aspirin in 0.1MHCl and calculate the total content of aspirin in the medium using
the declared content of aspirin.
Replace the 0.1MHCl in the vessel with 900ml of mixed phosphate buffer with a pH 6.8
previously held at 36.5 to 37.5 0C after 45 minutes take a sample from the medium and measure the
absorbance of suitable solution of aspirin in the dissolution medium and calculate the content of
aspirin in the medium using declared content of C9H8O4 in aspirin
DRUG PROFILE:

ODOUR: white crystalline or colorless.
MELTING POINT: 142 0C
BOILING POINT: 3190C
SOLUBILITY:3.3g/dm3 of water,142.9g/dm3 of acetone,50.0g/dm3 of ether.
STANDARD CURVE:
CONCENTRATION (mcg/ml) ABSORBANCE
0
2
4
6
8
10
DISINTEGRATION TABLE:
S.No Disintegration time(in sec)
DISSOLUTION TABLE:
Medium HCl buffer up to 45 min + MEDIUM 6.8 pH phosphate buffer
HCl buffer is replaced with phosphate buffer at 45 minutes
S.No
Time
(min)
Absorbance
Concentration
(µg/mL) D.F
%drug
Released
%drug
unreleased
Log%
drug-
unreleased
1 0
2 30
3 45
4 60
5 120
6 180
7 240
8 300
Report:

Expt no: 4
Date:
EVALUATION OF ANTACID PREPARATION
AIM: To find out acid neutralizing capacity of a commercial antacid preparation.
CHEMICALS:
Antacid tablet, Hydrochloric acid, Sodium hydroxide, Potassium hydrogen phthalate, Sodium
carbonate, Phenolphthalein indicator, Methyl red indicator.
APPARATUS: Mortar and pestle, conical flasks, burner, pipette, burette, burette stand.
PRINCIPLE:
Hydrochloric acid (HCl) is one of the substances found in the gastric juices secreted by the lining of
the stomach which is necessary for the digestion of the food. Acid is continuously secreted while
eating, consequently by taking excess of alcohol and food with spices lead to excess of stomach acid
which causes irritation on stomach lining particularly upper intestinal tract causing heart burn.
The most common bases used for over the counter antacids are:
Aluminium hydroxide, Al (OH)3 Magnesium hydroxide, Mg(OH)2
Calcium carbonate, CaCO3 Sodium bicarbonate, NaHCO3
Magnesium carbonate, MgCO3 Potassium bicarbonate, KHCO3
In this experiment antacids will be analyzed to determine the number of moles of acid neutralized per
tablet. The analytical procedure used is back titration. In this procedure, a known amount of HCl,
which is in excess, will be reacted with a weighed portion of a ground antacid tablet. The HCl
remaining after the antacid neutralization reaction occurs will be determined by titration with a
standardized NaOH solution to phenolphthalein end point. The number of moles of HCL neutralized
by the antacid (HCl neutralized) is the difference between the moles of HCl initially present in the
excess (HCl initial) and the moles of HCl titrated by the NaOH (HCl titrated).
HCl neutralized = HCl initial- HCl titrated

Procedure:
1. An antacid tablet was weighed and transferred in a clean mortar and the tablet was crushed
into a fine powder using the pestle.
2. About 0.2 grams of the ground up tablet was weighed and transferred into a clean 250 ml
conical flask. To this 25 ml of standard HCl solution (0.1M) was added.
3. The contents of the flask were warmed to dissolve the tablet. After the tablet dissolves the
solution was boiled for 1-2 min to remove the dissolved CO2.
4. 3-4 drops of the phenolphthalein indicator was added to the flask, and the excess HCl in the
solution was titrated by slowly adding standard NaOH solution to a phenolphthalein endpoint.
The no. of moles of HCl neutralized by the tablet can be calculated by the equation
N=A-B
Where A= No. of moles of HCl initially added to the tablet
A= (V HCl)(M HCl)
V HCl= Vol. of HCl (in litres) added to the tablet
M HCl= molarity of HCl solution
Where B= no of moles of NaOH required for back titration ( no. of moles of excess HCl)
B= (V NaOH)(M NaOH)
V NaOH= vol. of NaOH solution (in litres) required for back titrating excess acid.
M NaOH= Molarity of standard NaOH solution.
Acid neutralizing Capacity
Acid neutralizing capacity of antacid preparation can be calculated by the formula:
Acid neutralizing capacity=no. of moles of HCl neutralized/mass of tablet taken (gm)
Standardization of NaOH Solution:
Indicator: phenolphthalein (endpoint: Pink)
Molarity of hydrogen phthalate solution=
Vol. of NaOH solution consumed=
M1V1 = M2V2
M2=
Molarity of NaOH Solution=
Standardization of HCl:

Indicator: Methyl red (end point: faint pink)
Normality of sodium carbonate solution=
Vol. of HCl solution consumed=
N1V1=N2V2
N2=
Molarity of HCl Solution =
Analysis of Antacid:
S.No Contents in the flask
Burette readings (ml)
Vol. of NaOH
Consumed (ml)
Initial Final
1. Antacid sample + 25 ml HCl
2. Antacid sample + 25 ml HCl
The no. of moles of HCl neutralized by the tablet can be calculated by the equation
N=A-B
Where A= no. of moles of HCl initially added to the tablet
A= V (HCl) M ( HCl)
Where B= no .of moles of NaOH required for back titration (no. of moles of excess HCl)
B=V (NaOH) M (NaOH)
REPORT:
No. of moles of HCl neutralized, N=A-B
Acid neutralizing capacity=no. of moles of HCl neutralized/mass of tablet taken (gm)

The acid neutralizing capacity of commercial antacid tablet was found to be
Expt no: 5
Date:
FORMULATION AND EVALUATION OF ASPIRIN DISPERSIBLE
TABLETS AND COMPARISION WITH DISPRIN TABLETS
AIM: To formulate and evaluate Aspirin dispersible tablets and compare with commercial Disprin
tablets.
REQUIREMENTS:
APPARATUS: Hardness tester, Tablet punching machine, Roche friabilator, Dissolution apparatus,
U.V.Spectrophotometer, Disintegration, Electronic weighing machine.
CHEMICALS: Aspirin, Polyvinyl pyrrolidone, Sodium starch glycolate, Magnesium stearate, Talc.
PRINCIPLE:
Dispersible tablets are uncoated or film coated tablets that can be dispersed in liquid before
administration giving a homogenous dispersion. Dispersible tablets usually disintegrate within three
minutes when put in water or a small amount of breast milk. As for liquid formulations, the taste of a
dispersible tablet is a crucial parameter that will condition the acceptability by the child and the
adherence to treatment. Taste masking is obtained by adding flavours and/or sweeteners to the
formulation. Dispersible tablets have less physical resistance than regular tablets; they are most
sensitive to moisture and may degrade at higher humidity conditions. Each tablet must be protected
from the ambient humidity. Dispersible tablets must be used immediately after removal from the
blister packaging. Their stability outside of the blister cannot be guaranteed.
Aspirin is a non-steroidal anti-inflammatory drug which is poorly soluble in water. Aspirin dispersible
tablets are prepared by wet granulation method. The prepared formulations were passed the evaluation
test that is weight variations, percent drug content and disintegration, uniformity of dispersion,
hardness and friability.
Formulation of Aspirin dissolving tablets are advantageous over the conventional as they disintegrates
easily and enhancing fast dissolving their by fast absorption and fast onset of action, resulting in faster

exhibition of therapeutic responses. Hence these Aspirin rapid dissolving tablets are preferable than
conventional this also help to improve patient compliance.
DRUG PROFILE:
ODOUR: white crystalline or colorless.
MELTING POINT: 142 0C
BOILING POINT: 3190C
SOLUBILITY:3.3g/dm3 of water,142.9g/dm3 of acetone,50.0g/dm3 of ether.
PROCEDURE:
FORMULATION OF TABLETS:
The required quantity of Aspirin, Polyvinyl pyrrolidone (pvp-10%), were weighed in the beaker.
Sufficient quantity of ethyl alcohol was taken. Required quantity of Aspirin was dissolved in to
beaker containing ethyl alcohol. Dissolve PVP in beaker containing aspirin. There were mixed
thoroughly and kept in hot air oven at 90°C, for the evaporation of ethyl alcohol solvent. The damp
mass was passed through a sieve no: 16. The obtained granules were dried in hot air oven 60°C.The
obtained dried granules were again passed through sieve no: 16. Magnesium stearate passed through
sieve no: 120.Now Sodium starch glycolate (5%), Magnesium stearate (1%), Talc (2%) were added
one by one to obtained granules and mixed uniformly.
FORMULATION OF PARACETAMOL DISPERSIBLE TABLETS
INGREDIENTS QUANTITY FOR ONE TABLET QUANTITY FOR 20 TABLETS
Aspirin 350mg 7gms
PVP 30mg 600mg
Sodium starch Glycolate 15mg 300mg
Magnesium stearate 1.5mg 30mg
Talc 3mg 60mg
Total weight of each tablet= 400mg
STANDARD CURVE:
CONCENTRATION ( mcg/ml) ABSORBANCE
0
2
4
6
8
10
EVALUATION TESTS:
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 ----- mg and ----- mg each
for formulated and commercial tablet.
2. Wetting variation:
%deviation= (Each tablet weight-average weight)/Average weight*100
S.No Weight of the Tablet
Formulated Commercial
%deviation
(150mg-7.5%)
1
2
3
4
5
6
7
8
9
10
Average weight of tablet (mg) USP % difference
130/less 10
From 130 to 324 7.5
More than 325 5
3. HARDNESS: Hardness of tablets was determined by using Monsanto hardness tester. The lower
plunger was placed in contact with the tablets and zero reading was taken. The plunger was then
forced against a spring by tuning a threaded bolt until the tablet fractured as the spring was 5
compressed a pointer ridges along a gauge in the barrel to indicate the force 8.
Formulated=
Commercial=
4. FRIABILITY: The Roche friability test apparatus was used to determine the friability of the
tablets 20 per-weight tablets were placed in apparatus, which was given 100 revaluations. After
which the tablets were reweighed. The percentage of the friability was calculated.
Percentage friability= {(Initial weight- final weight)/Initial weight}*100
Formulated
Commercial
5. DISINTEGRATION TEST:

The disintegration test was carried out using the disintegration tester which consists of a
basket rack holding 6 plastic tubes, open at the top and bottom, the bottom of the tube covered by a
10-mesh screen. The basket was immersed in a bath of suitable liquid held at 37c, preferably in a 1L
beaker Tablets were placed in tubes and time taken by tablet to disintegrate was noted.
S.NO
DISINTEGRATION TIME (Sec)
Formulated Commercial
1
2
Dissolution test: Dissolution test were carried out to determine the amount of drug released during a
specific period of time using I.P apparatus-I (Paddle type).
Dissolution apparatus : Electro lab TDT 06L
Dissolution medium : 100ml of 0.1N HCl
Apparatus type : IP-1 (paddle type)
Speed : 50rpm
Sampling: 5ml of sample withdrawn at specific intervals of time (i.e. 5, 10, 15, 30, 45, and 60min)
and at each time fresh solution was replaced.
The obtained sample solutions optical densities were measured at maximum at about 249nm against
the blank using spectrophotometer. The absorbance values were noted.
Dissolution table of the formulated tablet
S.No Time Absorbance d.f. Concentration
(µg/ml)
%release %un
released
Log%
unreleased
1 0
2 5
3 10
4 15
5 30
6 45
7 60
Dissolution table of the commercial tablet
S.No Time Absorbance d.f. Concentration
(µg/ml)
%release %un
released
Log%
unreleased
1 0
2 5
3 10

4 15
5 30
6 45
7 60
TABLET
FORMULATED
COMMERCIAL
REPORT:
Expt no: 6
Date:
PREPARATION AND EVALUATION OF PARACETAMOL
DISPERSIBLE TABLETS
AIM: To prepare and evaluate paracetamol dispersible tablets.
REQUIREMENTS:
APPARATUS: Hardness tester, Tablet punching machine, Roche friabilator, Dissolution apparatus,
U.V.Spectrophotometer, Disintegration, Electronic weighing machine.
CHEMICALS: Paracetamol, Polyvinyl pyrrolidone, Sodium starch glycolate, Magnesium stearate,
Talc.
PRINCIPLE:
Dispersible tablets are uncoated or film coated tablets that can be dispersed in liquid before
administration giving a homogenous dispersion. Dispersible tablets usually disintegrate within three
minutes when put in water or a small amount of breast milk. As for liquid formulations, the taste of a
dispersible tablet is a crucial parameter that will condition the acceptability by the child and the
adherence to treatment. Taste masking is obtained by adding flavours and/or sweeteners to the
formulation. Dispersible tablets have less physical resistance than regular tablets; they are most
sensitive to moisture and may degrade at higher humidity conditions. Each tablet must be protected
from the ambient humidity. Dispersible tablets must be used immediately after removal from the
blister packaging. Their stability outside of the blister cannot be guaranteed.

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 that is weight variations, percent drug content and disintegration, uniformity of
dispersion, hardness and friability.
Formulation of Paracetamol dissolving tablets are advantageous over the conventional as they
disintegrates easily and enhancing fast dissolving their by fast absorption and fast onset of action,
resulting in faster exhibition of therapeutic responses. Hence these Paracetamol rapid dissolving
tablets are preferable than conventional this also help to improve patient compliance.
DRUG PROFILE:
STRUCTURE:
CHEMICAL NAME : 4-amino acetanilide
MOLECULAR WEIGHT : 151.2
MOLECULAR FORMULA : C₈H₉NO₂
CATEGORY : Analgesic, antipyretic
SOLUBILITY : Freely soluble in 95% ethanol and acetone,
Sparingly soluble in water,
Very slightly soluble in ether and dichloro methane.
PROCEDURE:
FORMULATION OF TABLETS:
The required quantity of Paracetamol, Polyvinyl pyrrolidone (pvp-10%), were weighed in the
beaker. Sufficient quantity of ethyl alcohol was taken. Required quantity of Paracetamol was
dissolved in to beaker containing ethyl alcohol. Dissolve PVP in beaker containing paracetamol
solution. There were mixed thoroughly and kept in hot air oven at 90°C, for the evaporation of ethyl
alcohol solvent. The damp mass was passed through a sieve no: 16. The obtained granules were dried
in hot air oven 60°C.The obtained dried granules were again passed through sieve no: 16.
Magnesium stearate passed through sieve no: 120.Now Sodium starch glycolate (5%), Magnesium
stearate (1%), Talc (2%) were added one by one to obtained granules and mixed uniformly.
FORMULATION OF PARACETAMOL DISPERSIBLE TABLETS
INGREDIENTS QUANTITY FOR ONE
TABLET
QUANTITY FOR 50
TABLETS
Paracetamol 120mg 6gms

Ethyl alcohol Q.S. Q.S.
PVP 15mg 750mg
Sodium starch Glycolate 7.5mg 375mg
Magnesium stearate 1.5mg 75mg
Talc 3mg 150mg
Total weight of each tablet= 150mg
PREPARATION OF PH 5.8 PHOSPHATE BUFFER:
Place 50ml of 0.2M potassium dihydrogen phosphate in 200ml volumetric flask, add 3.6ml of 0.2M
NaoH and then add water to final volume.
PREPARATION OF 0.2 M POTASSIUM DIHYDROGEN PHOSPHATE SOLUTIONS
27.218gms of potassium dihydrogen phosphate was dissolved in water and diluted with water and volume
was made up to 1000ml.
PREPARATION OF STANDARD STOCK SOLUTION:
100mg of paracetamol was accurately weighed and dissolved in ethanol and make up to 100ml using pH
7.8 phosphate buffer(1mg/ml).From this stock solution,2µg/ml,4,6,8,10µg/ml solutions were prepared and
measured the absorbance at 249nm using U.V.Spectrophotometer.
EVALUATION OF GRANULES:
BULK DENSITY: It is obtained by dividing the mass of the powder by the volume of the powder.
Bulk density = weight of powder in grams/bulk volume.
ANGLE OF REPOSE: It is the angle between the surfaces of the pile of granules on the horizontal
Surface.
Tan θ = h/r
Where, h=height of the heap
r= radius of the heap
ANGLE FLOW PROPERTY
25-30 Excellent
31-35 Good
36-40 Fair-aid not needed
41-45 Passable-may hang up
46-55 Poor-must agitate,vibrate
56-65 Very poor
>66 Very, Very poor
CARR’S CONSOLIDATION INDEX: It is the measure of potential strength that a powder could
build up in its arc in a hopper and also the ease with which such an arc could be broken.

Consolidation index = (Tapped density –Fluffy density)/Tapped density×100
HAUSNER RATIO:
H.R. = Tapped Density/Bulk Density
Compressibility Index (%) Flow Character Hausner’s 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
EVALUATION OF TABLETS:
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 ----- mg each for formulated
tablet.
2. Wetting variation:
%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
Average weight of tablet (mg) USP %difference
130/less 10
From 130 to 324 7.5
More than 325 5

3. HARDNESS: Hardness of tablets was determined by using Monsanto hardness tester. The lower
plunger was placed in contact with the tablets and zero reading was taken. The plunger was then
forced against a spring by tuning a threaded bolt until the tablet fractured as the spring was 5
compressed a pointer ridges along a gauge in the barrel to indicate the force 8.
Formulated=
4. FRIABILITY: The Roche friability test apparatus was used to determine the friability of the
tablets 20 per-weight tablets were placed in apparatus, which was given 100 revaluations. After
which the tablets were reweighed. The percentage of the friability was calculated.
Percentage friability= {(Initial weight- final weight)/Initial weight}*100
Formulated
5. DISINTEGRATION TEST:
The disintegration test was carried out using the disintegration tester which consists of a
basket rack holding 6 plastic tubes, open at the top and bottom, the bottom of the tube covered by a
10-mesh screen. The basket was immersed in a bath of suitable liquid held at 37c, preferably in a 1L
beaker Tablets were placed in tubes and time taken by tablet to disintegrate was noted.
S.NO DISINTEGRATION TIME (Sec)
1
2
6. Dissolution test:
Dissolution test were carried out to determine the amount of drug released during a specific
period of time using I.P apparatus-I (Paddle type).
Dissolution apparatus : Electro lab TDT 06L
Dissolution medium : 100ml of pH 7.8 phosphate buffer
Apparatus type : IP-1 (paddle type)
Speed : 50rpm
Sampling: 5ml of sample withdrawn at specific intervals of time (i.e. 5, 10, 15, 30, 45, and
60min) and at each time fresh solution was replaced. The obtained sample solutions optical densities
were measured at maximum at about 257nm against the blank using spectrophotometer. The
absorbance values were noted.
STANDARD CURVE OF PARACETAMOL (With pH5.8 Phosphate buffer at 257nm)
S.No CONCENTRATION (mcg/ml) ABSORBANCE
1 0.0

2 2.0
3 4.0
4 6.0
5 8.0
6 10
DISSOLUTION TABLE FOR FORMULATED TABLET
Time
(min)
Absorbance D.F
Conc.
(mg/ml)
%Drug
release
%Drug
unreleased
Log% Drug
unreleased
0
5
10
15
30
45
60
FORMULATED
TABLET
REPORT:
Expt no: 7
Date:
FORMULATION AND EVALUATION OF IBUPROFEN
SUSPENSION
AIM: To prepare and evaluate the Ibuprofen suspension
APPARATUS: Measuring cylinder, mortar and pestle, pH meter and Microscope
CHEMICALS REQUIRED: Ibuprofen, methyl paraben, acacia, amaranth red, glycerine, citric
acid, distilled water, sodium lauryl sulphate, strawberry, saccharine sodium.
PRINCIPLE: Ibuprofen is a non steroidal anti inflammatory drug (NSAID) that possesses anti
inflammatory, analgesic and anti pyretic activity. Its mode of action like that of other NSAID is not
completely understood but may be related to prostaglandin synthetase inhibition. Ibuprofen
suspension is sweetened, orange coloured, berry flavored suspension containing 100 mg ibuprofen in

5ml. Ibuprofen suspension is prepared by dispensing diffusible solid in a vehicle. Ibuprofen
suspension is mainly used as an antipyretic in pediatrics and for the treatment of rheumatoid arthritis
in adults. After the preparation of suspension, it is examined for the evaluation by conducting some
of the evaluation tests. This is the main principle involved in Ibuprofen suspension.
DESCRIPTION OF IBUPROFEN:
Ibuprofen suspension is a sweetened, orange coloured, berry flavored suspension containing 100mg
of ibuprofen in 5 ml suspension. The chemical name for ibuprofen is (±)-2-(p-isobutyl phenyl) prop
ionic acid.
DRUG PROFILE:
MOLECULAR STRUCTURE:
MELTING POINT: 74-770C
MOLECULAR FORMULA: C13H18O2
FORMULA:
S.NO INGREDIENTS QUANTITY
FOR 100ml
PURPOSE
1 Ibuprofen 2.5 g Active ingredient
2 Acacia 5% Thickening agent
3 Benzoic acid 2% Preservative
4 Citric acid 2% Buffering agent
5 Sodium lauryl
sulphate
1% Surfactant
6 Glycerin 2% Humectant
7 Amaranth red 2 ml Coloring agent
8 Strawberry 1 ml Flavoring agent
9 Sucrose 40% Sweetening agent
10 Water q.s Vehicle
PREPARATION OF IBUPROFEN SUSPENSION:

2 gm of Ibuprofen drug was weighed accurately and dispensed in mortar. All the remaining solid
ingredients like acacia and citric acid was added into the mortar and finely powdered them with the
help of a pestle. Accurately weighed quantity of sweetening agent was dissolved in sufficient
quantity of water and mixed it with remaining ingredients. Then add enough vehicles to make into a
smooth cream. Then add required quantity of amaranth red and flavouring agent and finally the
volume was made to 100ml by adding water by shaking the bottle. The prepared suspension was
evaluated by conducting evaluation tests.
EVALUATION OF IBUPROFEN SUSPENSION:
SEDIMENTATION VOLUME: Sedimentation volume (F) is nothing but the ratio of final volume
of sediment (Vu) to the original volume of sediment (Vo) before settling. 50 ml of each suspension
was transferred to 50ml measuring cylinder and the volume of sediment formed was noted for every
10 min up to 1 hr. The sedimentation volume (F) was calculated using the formula:
F=Vu/Vo
S.NO TIME (in min) Vo Vu F=Vu/Vo
1 0 100 100 1
2 10 100
3 20 100
4 30 100
5 40 100
6 50 100
7 60 100
Sedimentation volume(y axis) Vs time(x axis) graph was plotted.
REDISPERSIBILITY: The bottles containing suspension were held up right between the fingers
and rotated clockwise upside down through 180º in semicircular path and back in the anti-clockwise
direction. This process was repeated continuously until the sediment was completely redispersed.
pH MEASUREMENT: The pH of the prepared suspension was measured by using ELICO INDIA
pH analyzer (model L1612) by calibrating with standard buffers (pH 4.3 and 9).The pH of the
ibuprofen suspension was found to be

PARTICLE SIZE MEASUREMENT: The particle size of Ibuprofen particles in the prepared
suspension was measured by optical microscopy using a trinocular microscope at 100x (10x10)
magnification. The size of 100 particles was measured and the average particle size was determined.
CALIBRATION OF EYE PIECE SCALE:
1 division of stage micrometer= 0.01mm (10 µ)
X th division on stage micrometer= y th division on eye piece scale
th division on stage micrometer= th division on eye piece scale
So 1 division on eye piece scale=y/x*0.01mm
PARTICLE SIZE DETERMINATION:
Size Range (IN
µM)
MeanSize
Range
MeanOf Size
Range(Xl.C)
No Of
Particles(N)
%Frequency
(n)100//∑n
0-2 1 1.1
2-4 3 3.3
4-6 5 5.5
6-8 7 7.7
8-10 9 9.9
∑n=
REPORT:
Expt no: 8
Date:
FORMULATION AND EVALUATION OF IBUPROFEN
HYDROGEL
PRINCIPLE:
Hydrogels can be defined as colloidal gels in which drug particles are dispersed. Hydrogels
are formed by cross linking polymer chains through physical, ionic or covalent interactions. These
polymers are well known for their ability to absorb water. In most of the cases, they are

homogeneous materials and their bulk properties are characterized and considered with regard to
applications.
REQUIREMENTS:
Poly Vinyl Alcohol (PVA) - 7%w/v
Ibuprofen -100mg
Alcohol - qs
Distilled Water - qs
PROCEDURE:
PVA was soaked in water for 24 hrs. Then heated to 50 – 55°C and stirred to dissolve. The mixture
which is in solution at elevated temperatures and gel at room temperatures, Above mixture is cooled
to attain room temperature, and then the mixture of alcoholic drug solution (to dissolve the drug) was
added. The final mixture was subjected to freeze-thaw for three cycles. Freezing at -10°C and
thawing at 37°C. Finally a visco elastic gel was formed. The gel was subjected to evaluate for drug
content, consistency, pH, clarity and homogeneity.
EVALUTION TESTS:
Clarity:
The clarity of various formulations was determined by visual inspection under black and
white background.
Measurement of pH:
The pH of the gel formulation was determined by using pH meter. One gram of gel was dissolved in
100ml of distilled water. The measurement of pH of formulation was done.
Homogeneity:
All developed gels were tested for homogeneity by visual inspection after the gels have
been stored in the container for their appearance and presence of any aggregate.
Drug content:
500mg of gels was taken into a standard volumetric flask and dispersed in methanol.
Sample was withdrawn and the absorbance was measured at 254 nm and the drug content was
calculated from the calibration curve.
In vitro diffusion studies:
The in vitro diffusion study of prepared gel was carried out in Franz diffusion cell using
properly cleaned and washed chicken skin. 10ml of phosphate buffer was taken in a receptor
compartment, and then 100mg of ibuprofen gel (containing 10mg of drug) was spread uniformly on

skin membrane. The donor compartment was kept in contact with a receptor compartment and the
temperature was maintained at 37±0.5°C. The solution on the receptor side was stirred by externally
driven Teflon coated magnetic bars at predetermined time intervals, pipette out 3ml of solution from
the receptor compartment at specified time intervals for up to 2hrs and immediately replaced with
fresh 3ml phosphate buffer. The cumulative percentage release of drug was calculated against time.
STANDARD CURVE OF IBUPROFEN:
CONCENTRATION (µg/ml) ABSORBANCE
0.0
20
40
60
80
100
Drug dissolution profile by using Franz diffusion cell:
Time
(min)
Absorbance D.F
Conc.
(mg/ml)
%Drug
release
%Drug
unreleased
Log% Drug
unreleased
0
5
10
15
30
45
60
FORMULATED
GEL
REPORT:
Expt No: 9
Date:
QUALITY CONTROL TESTS FOR SALICYLIC ACID OINTMENT
AIM: To evaluate the quality control tests of salicylic acid.

DEFINITION: It contains 2%w/w of salicylic acid in a suitable water emulsifying basis.
EXRTEMPORANEOUS PREPARATION:
Salicylic acid finely sifted – 20g
Wool alcohol ointment – 980g
Melt the wool alcohol ointment gradually adds the salicylic acid and stir until cold. The ointment
complies with the requirements stated under topical semisolid preparation and with the following
requirements.
DRUG PROFILE
STRUCTURE :
MOLECULAR FORMULA: C7H6O3
IUPAC NAME: 2-hydroxy benzoic acid
CATEGORY: Keratolytic
DESCRIPTION: White or colorless or a white crystalline powder
MELTING POINT: 158-1610C
SOLUBILITY: Salicylic acid is freely soluble in ethanol (95%) and in ether, sparingly soluble in
chloroform, slightly soluble in water.
PROCEDURE:
STANDARDIZATION OF NaOH: 0.2g of potassium hydrogen phthalate was weighed and
dissolved in 100ml of water, from this 20 ml was taken and then add phenolphthalein as indicator.
The end point is colorless to pale pink.
PREPARATION OF 6M ACETIC ACID:
Solution of 6M acetic acid was prepared by diluting with 342ml of glacial acetic acid to 1000ml with
water.
PREPARATION OF IRON (III) CHLORIDE HEXAHYDRATE.
10.5% w/v solution of iron (III) chloride hexahydrate.
FORMULATION OF SALICYLIC ACID OINTMENT.
Required quantity of wool alcohol, white soft paraffin, hard paraffin & liquid paraffin are melted
together. It is then heated gently and stirred until it is cooled. 9g of wool alcohol was taken & melted

in this salicylic acid is add gradually and stirred until it becomes cool and made up to required
volume.
FORMULA: 10G OF OINTMENT
Salicylic acid finely sifted – 20g
Wool alcohol ointment – 980g
EVALUATION TESTS:
IDENTIFICATION:
Shake 1g with 10ml of water, filter and add to the filtrate iron (III) chloride solution R1; an intense
reddish violet color is produced which persists on the addition of 6M acetic acid. Add 2M HCl; the
color disappears and a white crystalline precipitate is produced.
ASSAY:
Dissolve 10g in a mixture of 20ml of ethanol (96%), previously neutralized to phenol red solution,
and 20ml of ether and titrate with 0.1M NaOH using phenol red solution as indicator. Each ml of
0.1M NaOH is equivalent to 13.81mg of C7H6O3.
CALCULATIONS:
Standardization of NaOH:
Molarity of Potassium Hydrogen phthalate = N1 =
Volume of Potassium hydrogen phthalate = V1 =
Molarity of NaOH = M2 =
Volume of NaOH consumed = V2 =
M1V1 = M2V2
M2 = M1V1/V2
=
1ml of 0.1M NaOH = 13.82mg of C7H6O3.
ml of M NaOH =
OBSERVATION & INTERPRETATION OF RESULTS:
Expt no: 10
Date:
FORMULATION AND EVALUATION OF DICLOFENAC SODIUM
TOPICAL GEL AND COMPARISION WITH COMMERCIAL GEL
AIM: To develop and evaluate topical Diclofenac sodium gel.
REQUIREMENTS:

CHEMICALS: Diclofenac sodium, HPMC, glycerin, distilled water.
APPARATUS: Volumetric flask, digital pH meter, UV – spectrophotometer.
PRINCIPLE:
For topical treatment of dermatological disease as well as skin care, a wide variety of vehicles
ranging from solids to semisolids and liquid preparation is available to clinicians and patients. Within
the major group of semisolids preparations, the use of transparent gels has expended both in
cosmetics and in pharmaceutical preparations. A gel is colloid that is typically 99% weight liquid,
which is immobilized by surface tension between it and a macromolecule network of fibers built
from a small amount of a gelating substance present. Topical drug is administration is localized drug
delivery system anywhere in the body through ophthalmic, rectal, vaginal and skin as topical route.
Skin is the one of the most readily accessible organs of human body for topical administration and
main route of topical drug delivery system. Number of medicated products is applied to the skin or
mucous membrane that either enhances or restore of a fundamental function of a skin or
pharmacologically alter an action in the underline tissue.
DRUG PROFILE:
 Molecular structure:
 Molecular formula: C14H11Cl2NO2
 Molecular weight: 328.1
 Chemical name: Sodium 2[2,6-dichlorophenyl)-amino] phenyl acetate.
 Category: Analgesic, anti inflammatory
 Dose: Orally or by intra muscular injection 25-75mg
 Description: A white to slightly yellowish crystalline powder
 Solubility: Freely soluble in methanol, soluble in ethanol, sparingly
soluble in water, partially insoluble in ether and chloroform.
PROCEDURE:
PREPARATION OF STANDARD STOCK SOLUTION: A 1mg/ml solution of drug was prepared
by dissolving 50mg diclofenac in 50ml of pH 6.8 phosphate buffer.
From this stock solution 2, 4, 6, 8, 10µg/ml solutions were prepared by diluting with pH 6.8
phosphate buffer. The absorbance was measured at 285nm and a graph was plotted between
concentration Vs absorbance.
PREPARATION OF GEL:
1g of diclofenac sodium was weighed and dissolved in 15ml of glycerin with the help of mild
heat (solution A). Weighed HPMC was added to the 75ml of distilled water and stirred until

dissolved (solution B). Solution A and B were mixed thoroughly and the final volume was made up
to 100ml.
EVALUATION OF POLYMER BASED GEL CONTAINING DICLOFENAC SODIUM:
The above formulated polymer based containing Diclofenac sodium was subjected to
evaluation for the following parameters
pH: The pH of gel formulation was determined by using digital pH meter.
HOMOGENEITY:
The prepared gel was tested for homogeneity by visual inspection after the gels have been set
in the container. They were tested for their appearance and presence of any aggregates
SKIN IRRITATION TEST:
Test for irritation was performed on human volunteers. Five volunteers were selected and
1.0g of prepared gel was applied on an area of 2 square inch to the back of hand. The volunteers were
observed for lesions of irritation.
DRUG CONTENT:
A specific quantity of developed gel was taken and dissolved in 100ml of phosphate buffer of pH
6.8 the volumetric flask containing gel solution was shaken for 2hr on mechanical shaker in order to
get complete solubility of the drug. This solution was filtered and estimated spectrophotometrically
at 285nm using phosphate buffer as blank.
FORMULA:
S.NO INGEREDIENTS QTY FOR 100g
1. Diclofenac sodium 1g
2. HPMC 3.5g
3. Glycerin 15ml
4 Distilled water Up to 100ml
STANDARD CURVE:
REPORT:
DRUG CONTENT
FORMULATED GEL COMMERCIAL GEL
mg/ml mg/ml
Exp no: 11
Date:
PREPARATION AND EVALUATION OF DICLOFENAC
INJECTION

AIM: To prepare diclofenac injection and evaluation of prepared and commercial diclofenac
injections.
CHEMICALS REQUIRED: Diclofenac sodium, Polysorbate 80 (MW 1310, Tween 80,
polyoxyethylene 20 sorbitan monooleate) occurs as a yellow oily liquid with a characteristic odor
and a warm, somewhat bitter taste. It has a specific gravity of 1.06-1.09 and a hydrophile: lipophile
balance (HLB) value of 15.0.5, ethylenediaminetetraacetate occurs as an odorless white crystalline
powder with a slightly acid taste. It is soluble 1 g in 11 mL of water and is slightly soluble in 95%
ethanol, Distilled water.
PRINCIPLE: Diclofenac sodium injection is commercially available. It is used in the treatment of
inflammatory diseases (rheumatoid arthritis, osteoarthritis, ankylosing spondylitis, juvenile arthritis),
dysmenorrhea and for its antipyretic effect. It is used topically in the treatment of actinic keratosis as
a 3% gel.
Diclofenac sodium (MW 318.13) is a phenylacetic acid derivative that is a nonsteroidal anti-
inflammatory agent with antipyretic activity. It occurs as a white to off-white, hygroscopic,
crystalline powder. It is soluble in ethanol and sparingly soluble in water. It melts at about 284°C. It
should be preserved in tight, light-resistant containers.
A known impurity is formed in the production of a parenteral dosage form of diclofenac sodium if
terminally sterilized by autoclave. This impurity has been detected as 1-(2,6-dichlorophenyl) indolin-
2one, which is also an intermediate from which diclofenac sodium is generally synthesized. It is only
the condition of the autoclave method (i.e., 123 +/- 2 °C) that enforces the intramolecular cyclic
reaction of diclofenac sodium forming the indolinone derivative and sodium hydroxide. The
formation of this impurity has been found to depend on the initial pH of the formulation. The
reaction follows first-order kinetics, and the energy of activation is 5.34 kcal/mol. The other
excipients in the formulation do not have a role in this reaction. It is thus preferable to use an
alternative sterilization method; that is, an aseptic filtration method in which the formation of this
impurity can be avoided. Terminal sterilization is done in order to determine whether the
formed impurity has any effect on drug content or not.
PROCEDURE:
1. This preparation should be done in a laminar airflow hood in a clean room or via isolation
barrier technology by a validated aseptic compounding pharmacist using strict aseptic
technique.
2. Calculate the required quantity of each ingredient for the total amount to be prepared.

3. Accurately weigh and/or measure each ingredient.
4. Add the polysorbate 80, alcohol and edetate disodium to about 75 mL of distilled water and
mix well.
5. Add the diclofenac sodium and stir until dissolved.
6. Add sufficient distilled water to volume and mix well.
7. Packed into glass vials with flame sealing and labeled.
8. The filled ampoules were terminally sterilized.
EVALUATION TESTS:
TEST FOR STERILITY:
The prepared injections were terminally sterilized in an autoclave. The sterilized injections were
subjected to test for sterility. One ml of sterile sample was collected from the ampoule in a laminar
unit and transferred to sterile casein digest broth and incubated at 370C. A positive control which was
inoculated with gram positive bacteria and a negative control without organism and sterile injection
sample were incubated at 370C. The sterility tests of commercial injections were also conducted.
DRUG CONTENT:
Approximately One ml of sterile sample of injection was taken and dissolved in 100ml of phosphate
buffer of pH 6.8 the volumetric flask. Drug content of the solution was estimated
specrophotometrically at 285nm using phosphate buffer as blank. It was compared with commercial
samples.
PARTICULATE MATTER: The terminally sterilized injection samples were visualized in the
light for the presence of particulate matter and compared with commercial samples.
STANDARD CURVE:
DRUG CONTENT TABLE:
S.No Sterilized injection
mg//ml
Commercial injection
mg//ml
Unsterilized Injection
mg//ml
1
Report:

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