KINGDOM OF SAUDI ARABIA
SALMAN BIN ABDULAZIZ
COLLEGE OF PHARMACY
PRACTICAL MANUAL
PHARMACEUTICS III
PHT-322
LEVEL VI
Lab Co-ordinator
Dr. Mohammad Khalid Anwer
Email:- m.anwer@sau.edu.sa
CONTENT OF LABORATORY EXPERIMENTS
Weeks Experiment
1
2
3
4
5
Send 20 gm of effervescent granules Sod.
Citrotartarate
7
To prepare and compress 30 tablets each
contains 0.9 g sodium chloride by direct
compression method
To prepare and compress 20, tablets each
contains sodium bicarbonate by wet
granulation method.
Evaluation of tablets
Evaluation of capsule dosage forms (B.P)
Preparation of glycerogelatin base
suppositories
9
10
11
Lab
Indiscipline
(-5)
Lab Record (5)
Preparation of absorbable dusting powder
Size reduction of camphor crystalline
powder by Pulverization by Intervention
method
Determination of Angle of Repose of
Powders
Determine the bulk density, porosity of 10
gm of the supplied powders A and B.
Provided that the true densities of
powders are 2.75 and 3.18 respectively.
Tabulate your results.
Determine the percent compressibility of
10 gm of magnesium sulphate powder by
calculating the tapped and bulk density.
Tabulate your results.
6
8
QC/Lab
discipline (5)
Note: All grading should be accompanied by signature of Lab instructor.
Note 2: Lab record must be checked on or before next experiment. (Late submission means
losing 1 grade/day)
Note 3: Final Lab exam (10) + viva/ synopsis/ other activities/ (5)
Lab Indiscipline (-5)
St Name Attendance
Late
entry
(-1)
No lab
Lab
Dirty
Dirty
coat
Indiscipline Workplace (-1) Glass wares (-1)
(-1) (-1)
EXPERIMENT - 1
AIM:- Preparation of absorbable dusting powder
Equipments required:Mortar and pestle, 90- mesh sieve, weighing balance
Rx
Corn starch
98 g
Light magnesium oxide
2g
Send 20 g
Sig.: to be used U.D.
Theory:Dusting Powders is used a medicated or non-medicated for external application for various parts
of the body as lubricants, protectives, absorbents, antiseptics, astringents and antiperspirants
agents. Dusting Powders are usually dispensed in sifter containers for convenient application to
the skin. Foot powders and talc powders are currently available as aerosols.
Procedure:1- Pulverize starch and magnesium oxide to fine powders, and pass through a 90-mesh
sieve.
2- Triturate the two powders (starch over magnesium oxide) in a mortar with pestle method
Use : As lubricant for surgical gloves.
Calculation :
Because of mechanical losses during preparation, you have to calculate for 25% excess so
, instead of preparing 20 g , you will prepare 25 g , the total amounts in the prescription is 100 g ,
so, multiply each ingredient by a factor of (25/100).
PRACTICAL LAB REPORT:AIM:-
Calculations:-
Results/ Observations:-
Uses of each ingredients: -
Indications:-
EXPERIMENT - 2
AIM:- Size reduction of camphor crystalline powder by Pulverization by Intervention
method.
Equipments required:Mortar and pestle, weighing balance
Materials required:Camphor crystals, Alcohol.
Theory:It is the reduction of particle size with the aid of a second agent which can be readily removed
from the pulverized product.
This is the process of reducing the state of solids with the additional material as volatile solvents
which can be removed easily after the pulverization has been completed and the powdered
material is obtained. This technique is applied to substances which are gummy and tend to
reagglomerate or which resist grinding.
Procedure:1. Weigh 1g of camphor crystal
2. It is readily triturated when a few drops of alcohol or other volatile solvent is added.
3. The pulverized camphor is readily recovered as the solvent evaporates.
PRACTICAL LAB REPORT:AIM:-
Calculations:-
Results/ Observations:-
Uses of each ingredients: -
Indications:-
EXPERIMENT - 3
AIM:- Determination of Angle of Repose of Powders
Equipments Required:-Funnel, Funnel stand
THEORY:Flow of powders
One of the properties which are of great concern to pharmacists is the extent to which free
flow will occur.
Many pharmaceutical processes require free flowing powders. Such requirements include the
following:
1- The control of weight in both capsules and tablets is dependent upon the reproducibility of
powder flow into fixed volumes receptacles.
2- Powders that are too fluid are difficult to hand pack into cap sules.
3- Dusting powders must be free flowing to facilitate delivery. Through the sifter caps and
spreading applied to the body.
4- Poorly flowing cohesive powders are also difficult to blend uniformly.
The majority of powders are not free flowing unless specially treated to make them more
flowable.
PROCEDURE:In this procedure we will measure the flow characteristic of some powders of pharmaceutical
interest. And study the effect of glidants on the flow characteristics of various powders.
1. A quantity of powder is allowed to flow through a funnel , whose tip is adjusted at 2 cm
form a horizontal surface beneath , so that the apex of the heap just touch the lower tip of
the funnel.
2. Mark the base of heap.
3. Remove the powder.
4. Measure the diameter of the formed circle (take the average of two diameters).
5. Repeat the process three times and calculate the average diameter (d ) , and the radius r =
d / 2.
6. The height of the heap ( the distance between the horizontal surface and the lower tip of
the funnel is called ( h ).
7. Tan the angle of repose ( Ø ) = h / r , get Ø , and tabulate your results.
Relationship between angle of repose and powder flow
Angle of Repose (θ)
< 25
25–30
30–40
> 40
Flow
Excellent
Good
Passable
Poor
PRACTICAL LAB REPORT:AIM:-
Calculations:-
Results/ Observations:Observation Table:-
Powders
Sodium chloride
Lactose
Sodium chloride +
2% talc
Lactose + 2% talc
Height of heap
(h)
Radius (r)
h/r
Angle of Repose
(Ø)
Experiment - 4
AIM:- Determine the bulk density, porosity of 10 gm of the supplied powders A and B.
Provided that the true densities of powders are 2.75 and 3.18 respectively. Tabulate your
results.
Theory:-
Density of Powder:Density is define as weight per unit volume
1- True density of the material itself
2- Bulk density: was determined from the bulk volume and the weight of a dry
powder in a graduated cylinder. The bulk density is sometimes given for both
loosely packed powder and tightly packed powder.
The method of measuring bulk density
It involves introducing a known weight of the material into a graduated cylinder
and compacting the powder by a standardized procedure.
3- Tapped density: Tapped volume is measured by weighing certain amount of particles
and carefully introduces it into a 100cc graduate cylinder. The cylinder is dropped
into a hard surface until a constant volume was obtained. From the used weight and
the obtained volume the tapped density was calculated. Tapped density provides
information on how closely the particles in the powder have packed together as a result
of tapping or compression.
Porosity:Porosity is defined as the ratio of the total volume of space between the particles to the
bulk volume of the packing. The porosity of powder is given by:
Vb is the bulk volume and Vt is the true volume of the powder. Porosity is
frequently expressed in percent (%)
PRACTICAL LAB REPORT:AIM:-
Calculations:-
Results/ Observations:-
Experiment - 5
AIM:- Determine the percent compressibility of 10 gm of magnesium sulphate powder by
calculating the tapped and bulk density. Tabulate your results.
THEORY:Determination of Compressibility of Powder:
Powders used for tabulating should possess good compressibility percent less than 22 %
considered to have good flow ability.
The compressibility percent (c) was calculated according to the following equation
Where Pt and PB are the tapped and bulk densities respectively
PRACTICAL LAB REPORT:AIM:-
Calculations:-
Results/ Observations:-
Granules
Granulation is a method for, improving the flow ability of powder drugs. It include the
converting the powder of the drug into agglomerates of smaller particles (free flowing coarse
powder) to be administered as such or to be tabulated or encapsulated. Granulation also allows
the addition of flavoring and coloring agents and produces an easily handled, attractive, palatable
product.
Granules can be prepared in different forms:
1.Non- effervescent granules that contain in addition to the drug other additives such as sugar,
lactose, starch .... etc. All ingredients are moistened and made as a wetted mass with a
granulating agent such water, starch mucilage, gelatin and sucrose solutions or dilutions of
alcohols. The mass is then pressed through a sieve of appropriate size and the resulting granules
dried. The granules should be uniform in size as possible.
2. Effervescent granules
That effervesce on addition to water, and usually contain mixture of citric, tartaric acids with
bicarbonate soda and usually some medicaments and occasionally sugar. They are dissolved in
water for purposes of administration and taken during effervescence or immediately thereafter.
3- Coated granules
That may be coated with film of polymeric material in order to control the release of the drug
after swallowing.
1- Effervescent granules:
The effervescent granules are popular in use due to the pleasant taste of carbonated solution and
to psychological effect.
A mixture of acids will be used because tartaric acid produces a chalky friable granules and citric
acid is too sticky to be manipulated. It is desired that citric acid and tartaric acid are to be used
in the ratio of 1:2 respectively.
Rx
Citric acid
1
Tartaric acid
2
Sodium bicarbonate
3.4
6.4
For preparation of effervescent granules, citric acid should be powdered just prior to use. Sodium
bicarbonate should be powdered and dry. Other ingredients should be dried to 100°C until they
cease to loss weight. All ingredients should be passes through sieve No. 60. The effervescent
mixtures of this kind react very rapidly when added to water and in many cases part of the
draught is lost due the violence of the effervescence.
Method of Manufacture;
The preparation of effervescent granules on either small or large scale. More or less the same
general procedures which are:
1- Preparing formula
2- Mixing the ingredients
3- Moistening and granulating
4- Drying the moist granules ate 50-60 °C
5- Packing and storing.
6- The amount of medicinal agent should be determined according to the dose desired.
The usual procedure for the physician is to prescribe a teaspoonful dose or multiple
of that amount A heaping teaspoonful of an effervescent salt weighs 5 gm. If the
dose of the medicament is 0.5 gm, then the finished product should contain 4.5 of
the effervescent salt mixture to each teaspoonful.
Two methods for the preparation of effervescent granules are
 Fusion method
 Wet methods.
Wet Method:
1- Finely powder all of the ingredients and pass each separately, thorough sieve No. 60.
2- Mix the powder homogenously in a porcelain dish
2- The mixture of the powdered materials is massed with 95% alcohol until dough is obtained.
3- The so-produced mass is granulated in a likewise manner as described above.
Evaluation of the granules:
The quality control tests of effervescent granules is carried out to Determine
I- Effect of methods of preparations
II- Effect of granules Size
I -Effect of methods of preparations
1- An accurately weighed 0.25 gm of the granules and the transfer into a dry clean measuring
cylinder (100 ml capacity).
2- Add 5 ml of distilled water to the granules and record the following:
a-The time lapsed before effervescence is recorded.
b- The volume of the produced CO2
c-The time required until effervescence ceases.
d- The clarity of the solution after effervescence
completely ceases.
e- The Evaluation tests are better carried out on the
granules prepared by the two methods (Fusion
and Wet methods) and the results are tabulated
for comparison .
II- Effect of granules Size
1- Prepare 50 gm of effervescent granules (adopt the general procedure of moist granulation
technique ) and the passed through
a- Sieve No. 10 (2000 µm)
b- Sieve No. 20 (840 µm)
c- Sieve No. 40 (420 µm)
The pervious quality control testes are carried out and the result are tabulated in the fallowing
table:
Experimental Work
(1)
Uricosuric Effervescent granules
(Non-medicated Granules)
Send 20 gm of effervescent granules containing
20% of - Magnesium sulfate (Mg SO4),
- Magnesium carbonate ( MgC03)
- or magnesium oxide (Mg 0)
Experiment – 6
AIM:- Send 20 gm of effervescent granules Sod. Citrotartarate.
Equipments required:Mortar and pestle, weighing balance, sieve.
Materials required:Citric acid, Tartaric acid, Sodium biocarbonate, Sucrose
RX
Sodium bicarbonate
510 gm
Citric acid
180 gm
Tartaric acid
270 gm
Sucrose
150 gm
Send
20 gm
Calculations
Calculate for 25
Procedure:
1- All the ingredients are finely powdered and passed through sieve No. 60.
2- Magnesium sulfate must be exsiccated by heating in a clean dry porcelain dish on directflame till completely dry.
3- The powders are mixed homogenously, massed with 95% ethanol. The produced dough is
passed through a sieve No. 10.
4- The resultant granules are dried in hot air oven at 40 °C for 4 hours.
PRACTICAL LAB REPORT:AIM:THEORY:-
Calculations:-
Results/ Observations:-
Evaluation of the granules:-
Uses of ingredients:-
Tablets
A compressed tablet is unit dosage form prepared by compression under several hundred
kilograms of pressure per square centimeter, granulated medicinal or powdered substances
into a, discoid shape by means of dies. Tablets usually consist of several materials in addition
to the medicament that they convey to the patient. These components have different
functions. Although all of them furnish bulk or volume to the tablets, they are usually
classified according to the principle function in the tablet. Therefore. The word diluent "or"
bulking agent applies only to those substances that usually make up the major portion of the
tablet. Substances that bind powders together and make then cohesive are the "binders".
Tablet Ingredients :
Materials that help the tablet to break up and dissolve to release the medicament are
the disintegrates. In order for granules to flow from a hopper on the tablet press to the die
and for consistent and uniformly fill, substances called "glidants" are added to the formula.
Once the tablet has been compressed, it will not release from the die unless a "Lubricant' is
present in sufficient amount. Sometimes the compressed tablet leaves a film on the Punches
and "anti-adhesives" are needed to prevent this. The last three substances frequently have
interrelated properties. Ingredients sometimes added but not essential for tab letting are dyes,
flavors, sweetness, adsorbents, and buffers.
Compressed tablets
A compressed table is a unit dosage form _prepared by compressing medicinal substance in
a powder or granular form under several hundred kilograms of force per square centimeter into the
required shape by means of punches and dies. There are approximately 360 official tablets.
Tablets usually consist of several materials in addition to the drug called excipients
These excipients are classified according to their principle function they exert in the tablets.
I- Diluenis , Bulking agents, Fillers:
These are substances inert and stable used to increase the
volume of the tablet.
Soluble: eg Lactose, sucrose, mannitot sorbitoL
Insoluble: eg Calcium sulfate, dicalcium phosphate ,
tricalcium phosphate starch calcium carbonate .
2 - Binders or AdhesivesThese are substances that bind all the powder together to make them as cohesive paste. Binders may be
added in a dry or in solution form. Binders are either polysaccharides polymeric materials.
Examples of binder used
- Acaciamucilage
10-20%
-Tragacanth mucilage
10-20%
- Gelatin solutions
- Starch mucilage
3-10%
5-10%
- Glucose syrup
25-50%-67%
Cellulose derivatives
3-10%
3- Disintegratents:
These are materials that help tablet break up into small particles in the gastrointestinal tract.
Examples :
Starch, alginates, cellulose derivatives, and lactose
Disintegrates added into tablets in two portions.
- One half is added to the powdered components before
the wet granulation process
- Second half added to the finished granulation just prior
to compression.
5- Lubricants
-
These are agents that reduce the friction between the tablet edges and die wall during the
ejection cycle. They are usually added at the very last step before compression. They present
on the granules surfaces and in between them and the Parts of the tablet press.
-
Example: Magnesium stearate, stearic acid, talc.
6-Glidants are Materials that improve the flow characteristics of
granulation. Example:- Talc
7-Anti- adherents: Are materials used to prevent tablet sticking to the faces of ft punches and
die walls. Example: Talc.
8- Other table components
These are coloring agents, flavors, sweeteners and
adsorbents. etc.
Manufacture of compressed tablets
For tablets manufacture fine powders are the basis of most formula. But they do not flow
easily and are difficult to feed into the die and they will not easily binder under
compression. If however, this fine powder is converted into granules by granulation
(pretreatment).
Granulation is the process the fine powders are converted to granules using either Wet
granulation or Dry granulation that improve flow ability of powder to ensure a uniform
fill of the die cavity.
Experiment - 7
AIM:- To prepare and compress 30 tablets each contains 0.9 g sodium chloride by direct compression
method.
Rx
Sodium chloride
0.9 g
Equipments required:Weighing balance, sieve, tablet punching machine.
Note:1- The crystals of sodium chloride are granular and free
Flow able (No need for granulation)
2 - Sodium chloride crystals when compressed, bind together,
To produce tablets of good hardness (no need for binding
Agent)
3-Tablets of sodium chloride, being soluble tablets (no need for disintegrating agent)
4-Sodium chloride when compressed, dose not stick to metal of punches and dies of tablets machine
(no need for lubricant).
Procedure:
1- Screen sodium chloride crystals through a No. 16-22 sieve. This step is necessary to break down
lumps and to produce a uniform granular powder.
2- Adjust the tablet machine to 1/2 gm size tablet.
3- Fill the sodium chloride into the feeder (hopper) of tablet machine whose dosing unit
has been adjusted for compressing tablets having weight 0.5 gm. Check on the weight of
the tablets every now and then adjust the machine accordingly.
PRACTICAL LAB REPORT:AIM:THEORY:-
Calculations:-
Results/ Observations:-
Uses of tablets:Tablets used in preparation of isotonic solutions
One tablet dissolved in sufficient water for injection and the volume completed to 100 ml.
Label:
Storage:
Store in well closed container.
Experiment - 8
AIM:- To prepare and compress 20, tablets each contains sodium bicarbonate by wet
granulation method.
Rx
Sodium bicarbonate
300 mg
Peppermint Oil
0.003 ml
Acacia powder
3%
Acacia mucilage
q.s (25%)
Magnesium stearate
0.25% 0.75%
Talc purified.
Procedure
1. Acacia mucilage is prepared by dissolving 5gm of powdered acacia in 10 ml. of water and
stirring until the acacia is dissolved then complete to 20 ml warm water.
2. Sodium bicarbonate mixed with powdered acacia.
3. The pervious mixture moistened with the acacia solution.
4. Wet mass is pressed through a sieve 0.84 mm.
5. Granules are dried at temperature not exceeding 60°C and sieved to remove powder and
small granules.
6. Peppermint oil is added. The oil is dissolved in little alcohol and sprayed on the dry
granules, which are continually turned over during the process.
7. Finally, lubricants are added and the whole are shaken in a dry way.
8. Granulation is transferred to the hopper of tablet machine adjusted for compression of
tablets having calculated final compression weight.
PRACTICAL LAB REPORT:AIM:THEORY:-
Calculations:-
Results/ Observations:-
Use of tablets:Used as gastric antacid, in treatment of systemic acidosis. It can be used locally on the skin in the form
of moist paste or solution. In this form, it is an effective antipruritic.
Label:
Storage:
Store in well closed container.
Experiment – 9
AIM:- Evaluation of Tablets
Tablets are evaluated by a variety of methods.
A)
Unofficial Tests :
1.Tablet hardness
The tablets must be hard enough to withstand mechanical stress during packaging, shipment, and
handling by the consumer. Section <1216> of the USP 24/NF19 outlines a standard tablet
friability test applicable to manufactured tablets. Most compounding pharmacy would not have
the apparatus specified in Section <1216>. However, there are several hand operated tablet
hardness testers that might be useful. Examples of devices are the Strong Cobb, Pfizer, and
Stokes hardness testers. The principle of measurement involves subjecting the tablet to an
increasing load until the tablet breaks or fractures. The load is applied along the radial axis of the
tablet. Oral tablets normally have a hardness of 4 to 8 or 10 kg; however, hypodermic and
chewable tablets are much softer (3 kg) and some sustained release tablets are much harder (1020 kg).
Experiment :Determination of Tablet Hardness
Using a hardness tester ( Erweka ) , determine the hardness of the four (4) different types of
tablets supplied. Use an average of three measurements for each determination and comment on
your results.
Hardness Tester _______________
Tablet Type
Hardness 1
Hardness 2
Hardness 3
Mean Hardness
Comment on Results :
2. Friability Test:
•
Measurement of Friability : This test is designed to measure the ability of the tablet to
withstand handling and transportation.
Procedure : ( using Roche Friabilator ) :
1.
Take 20 tablets dedust and weigh them (wo)
2.
Place tablets in friability drum , switch on the apparatus adjusting the timer to 4 min. ,
and the speed at 25 r.p.m.
3.
At the end of the operation the tablets are removed , de dusted and re- weighed (w) .
should any tablet break the batch is rejected .
4.
Friability B is expressed as a percentage loss in weight :
B =100 (1 - (w/wo ) )
5.
If value of B is 1.0 % or less , the batch is accepted .
B) Official Standards(U.S.P.)
I ) Uniformity of Dosage Units :
Analytical determination of tablet content:
This probably will not be done due to the requirement of specialized equipment. However, the
weight variation of the tablets can be measured by weighing each individual tablets and
determining the percent difference from the intended amount. Guidelines in the USP 24/NF19
Supplement 1 indicate that each tablet "shall be not less than 90% and not more than 110% of the
theoretically calculated weight for each unit."
Experiment : Determination of Weight Variation:
The total weight of a tablet is determined by the depth of the die cavity, bulk density of granules
or powder, and uniformity of particulate flow. Even with a proper granulation having uniform
flow, a volume fill is not as accurate as a fill based on weight. Therefore, tablet weight variations
must fall within certain specifications established by the USP.
Tablets are required to meet a weight variation test where the active ingredient comprises a
major portion of the tablet , tablets containing 50 mg or less of active ingredients , comprising
less than 50% by weight of the tablet should pass a content uniformity test.
Procedure :
Select 30 tablets and proceeds as follows ;
1)
Weigh accurately 10 tablets individually and calculate the average weight .
2)
Calculate the average value of drug content as % following the assay procedure using
another sample obtained from the same batch .
3)
Calculate the relative standard deviation (RSD)
[ Note : use excel program ]
Tablet #
1
2
3
4
5
6
7
8
Weight of Tablet (mg)
% Labeled Claim
9
10
Note: Labeled claim is 750 mg
•
Mean (as % of labeled claim) _________
•
Standard Deviation __________
•
RSD __________
( Assay procedure of Aspirin tablets : )
Powder 10 tablets , weigh 0.5 g of powdered tablets , put in conical flask , add 25 ml of 0.5 N
NaOH , boil gently for 5 min. , cool and titrate excess alkaline with 0.5 N HCL using phenol red
as indicator
-
Each ml of 0.5 N HCL is equivalent to 0.045 g Aspirin
-
Repeat the operation without aspirin
-
Amount of Aspirin = ( B – Exp. ) x 0.045 = A
-
% of Aspirin in tab. =( A / 0.5 ) x 100
(average content )
4)
Calculate the content of active ingredient
in each 10 tablets = tab. Wt. X average content
100
•
Determination of Content Uniformity:
NOTE: Tablets should be analyzed in the same order as the weight variation test so that a
comparison between weight variation and content uniformity can be made.
Determine the content of active ingredient of the tablets by the procedure given below.
-
Select 30 tabs and proceed as follows :
Assay 10 tablets individually as directed in the assay in the individual monograph unless
otherwise specified in the test for content uniformity
-
Calculate RSD as before.
Criteria : ( apply the following criteria , unless otherwise specified in the individual monograph )
A)
If the average of the limits specified in the potency definition in the individual
monograph is 100 % or less :
For weight variation , or content uniformity :
The requirements are met if the amount of the active ingredient in each of 10 tablets tested
lies within the range of 85 % to 115 % of the label claim and relative standard deviation is less
than or equal to 6.0% .
If one tablet is outside the range of 85% to 115 % of the label claim and no tablet is outside
the range of75 % to 125 % of the label claim or if RSD is greater than 6 , or if both conditions
prevail , test 20 additional units the requirements are met if not more than one tablet of the 30 is
outside the range of85 % to 115 % if the label claim and no tablet is outside the range of 75 % to
125 % of the label claim and RSD of the 30 tablets does not exceed 7.8 % .
B)
If the average of the limits specified in the potency definition in the individual
monograph is greater than 100 % :
1.
.
If the average value of the tablets tested is 100 % or less , The requirements are as in (A)
2.
If the average value of the tablets tested is greater than or equal to the average of the
limits specified in the potency definition in the individual monograph , the requirements are as in
(A) . except that the word s “ label claim “ are replaced by the words “label claim multiplied by
the average of the limits specified in the potency definition in the individual monograph is
divided by 100 “ .
If the average value of the tablets tested is between 100 % and the average of the limits specified
in the potency definition in the individual monograph , the requirements are as in (A) , except
that the word s “ label claim “ are replaced by the words “label claim multiplied by the average
value of the tablet tested ( expressed as % of label claim ) divided by 100 “
Experiment : Tablet disintegration :
Disintegration is an essential attribute for tablets intended for administration by mouth , except
those intended to be chewed before being swallowed and except some types of sustained release
tablets.
Disintegration (for un-coated tablets )
This test is provided to determine compliance with limits on disintegration stated in the
individual monograph . Disintegration does not imply complete solution of the tablet or even its
active constituent .
Complete disintegration is defined as that state in which any residue of the tablet remaining on
the screen of the test apparatus is a soft mass having no palpably firm core.
Procedure:
1.
Place one tablet in each of the six tubes of the basket , add a disk to each tube
2.
Operate the apparatus , using water maintained at (37+2) o C . as the immersion fluid
unless another fluid is specified in the individual monograph .
3.
At the end of the time limit specified in the individual monograph , left the basket from
the fluid ,and observe the tablets : all of the tablets have disintegration completely . if one or two
tablets fail to disintegrate completely , repeat the test on 12 additional tablets : not less than 16 of
the total of 18 tablets tested disintegrate completely .
Apparatus : refer to USP for details.
II)
Tablet dissolution :
Disintegration time determination is a useful tool for production control, but disintegration of a
tablet does not imply that the drug has dissolved. A tablet can have a rapid disintegration time
yet be biologically unavailable. The dissolution rate of the drug from the primary particles of the
tablet is the important factor in drug absorption and for many formulations is the rate-limiting
step. Therefore, a dissolution time is more indicative of the availability of a drug from a tablet
than the disintegration test. Even though this is an important parameter to measure.
Place the stated volume of dissolution medium in the vessel of the apparatus specified in the
individual monograph, assemble the apparatus, equilibrate the dissolution medium to 37 + 0.5 o
C and remove the thermometer. Place one tablet in the apparatus, and operate at the specified
rate of the monograph. At the time specified, withdraw a sample and perform the analysis as in
the monograph. Repeat the test with additional tablets.
Unless otherwise specified in the individual monograph and the requirements are met if the
quantities of active ingredient dissolved from the tablets tested conform to the accompanying
acceptance table.
ACCEPTANCE TABLE
Stage
Number
S1
6
S2
6
S3
12
Tested
Acceptance Criteria
Each Tablet is not less than Q + 5%
Average of 12 tablets (S1+S2) is equal to or greater than Q, and no unit is less than Q-15 %
Average of 24 tablets (S1+S2+S3) is equal or greater than Q and not more than two tablets are
less than Q-15%
Continue testing through the three stages unless the results conform at either S1 or S2. The
quantity Q, is the amount of dissolved active ingredient specified in monograph expressed as a
percentage of the labeled content. Both the 5% and 15% value in the acceptance table are
percentages of the labeled content.
Dissolution Test For Aspirin Tablets (Uncoated)
- Medium :
-
0.05 M acetate buffer having pH of 4.5; 500ml
Time : 30 min , Q : 75 %
Assay Procedure :
1)
At the time specified, 2 ml aliquot is pipetted out through a Millipore filtration unit and
placed in a 50 ml volumetric flask. Then add 2 ml dissolution medium to the dissolution vessel.
2)
After adjusting volume to 50 ml with 0.1N sulfuric acid, the absorbance of each solution
is measured at 228 nm.
3)
The amount of Aspirin dissolved ( C ) =
(Absorbance X Conc. Factor X Dil. Factor X Dissolution Medium Volume) = (Absorbance X
0.02 X 25 X 500 ) mg.
4)
Percentage of Aspirin dissolved at time specified =
5)
C/ Label Claim X 100 = C/325 X 100
Dissolution Apparatus :
Capsules
Capsules are shells of gelatin with individual dos medications. They provide accurate dosage of drugs and
mask their bitter taste. When swallowed the gelatin shell dissolves in the G.I fluid and release its content within
5 minutes. Capsules are gelatin filled with powdered drug blended with other ingredients that make up an
individual dose. Dry powders, semisolid, and liquids that do not dissolve gelatin may
be encapsulated.
- Soft Gelatin capsules:
These are formed, filled and sealed in one manufacturing operation and may contain
powders, non-aqueous liquids, solutions, emulsions, suspensions and pastes .
- Hard gelatin capsules :
The shell is manufactured from gelatin with the addition of suitable plasticizers,
preservatives and coloring agent. Hard gelatin shells are available in a range of sizes.
The hard gelatin capsules consists of two closely fitted cylinders each
having a closed and open end .
a-The lower cylinder is called the body or base,
b-The upper cylinder called Cap.
Method of filling hard gelatin capsules :
With dry materials.
1- P r e p a r i n 2 t h e m a t e r i a l .
All the substances are reduced by trituration to about the same particle size and then mixed by the
process of geometric dilution. Powders that flow easily and those that creep when triturated may be
filled into capsules more easily if they are wetted with a drop or two of a liquid. Alcohol is
the liquid of choice, but water or mineral oil might also be used.
2- Choice of an appropriate capsule size.
The capsules, that is convenient to the prescribed dose is selected. Smallest is selected as the bigger
present difficulty in swallowing.
Approximate capacities of hard gelatin capsule shells
Filling by hand
Weigh each capsule as it is filled. The cap is removed and the powder is transferred into the body, then cap is
the slipped into its place and weight tested in compression with an empty one.
Cleanliness
As any trace of moisture can make capsules sticky and cause dry powders to adhere and leave finger prints. So
hands must be clean and dry. This can be achieved by the following methods:
I- Rub hand with towel before filling of each capsule
2- Use the cap of another capsule as a holder for the base (body) during filling.
3- Wear finger cots or rubber gloves.
Determination of the capsule fill weight
To determine the size of the capsules to be used or fill weight for formulation, the
following practical relationship is used:
Fill weight = tapped density of formulation x capsule volume
1- Example (if the size of capsule fit with the standard
capsule size.
A formulation has a theoretical fill weight of `350 mg and a tapped bulk density of 0.75 g/ml
What size capsule is required?
Volume occupied by fill capsule = 0'35/0.75 = 0.47 ml.
It can be seen from the above table that a size 1 capsule has a volume of 0.48 ml. so it is the required size for the
particular formulation.
2 Example (if the size of capsule dose not fit with the standard -capsule size.
A preliminary mixture has a fill weight of 500 mg and a tapped bulk density of 0.80 g/ml.
Volume occupied by fill weight = 0.5/0.8 = 0.63 ml.
It can be seen that capsule size 0 can be used (size 0 = 0.67 ml) .
The difference 0.67-0.63 =0.04
showed that there is 0.04 ml unoccupied
To solve this problem we can add diluent to the mixture to
improve it performance.
Weight of diluent = 0.04 x 0.8 = 32 mg
32 mg diluent + 500-mg mixture weight = 532
= 0.532 g/0.8 = 0.67 ml
EXPERIMENT - 10
AIM:- Evaluation of capsule dosage forms (B.P)
Disintegration test: The disintegration test determines whether tablets or capsules disintegrate within a
prescribed time when placed in an aqueous medium under the prescribed experimental
conditions.
 Disintegration is the state in which no residue, except fragments of capsule shell, remains
on the screen of the test apparatus or adheres to the lower surface of the disc, if a disc has
been used.
 Method:1. Introduce one capsule into each tube and suspend the apparatus in the beaker containing
water.
2. If the hard capsule floats on the top of water, the disc may be added.
3. Operate the apparatus. Record the time. Remove the assembly from the liquid. The
capsules pass the test if no residue remains on the screen of the apparatus.
4. The capsules should disintegrate within 30 minutes, unless otherwise justified.
2. Uniformity of weight: This test is to be done on 20 capsules.
Method:
1. Weigh an intact capsule.
2. Open the capsule without losing any part of the shell and remove the contents as
completely as possible. Weigh the shell.
3. The weight of the contents is the difference between the two weightings.
4. Repeat the procedure for further 19 capsules selected at random.
5. Determine the average weight.
6. Compare the average weight to the table below, to determine the % deviation permitted.
7. Calculate the upper and lower limits at the % deviation stated, and at double that
percentage.
8. Compare the individual weights of the capsule contents to the upper and lower limits
calculated at the % deviation stated, and at double that %.
9. Limit: not more than two capsules of the individual weights deviate from the average
weight by more than the % deviation listed in the table, and none deviates by more than
twice that %.
Average weight of
capsule content (mg)
% deviation
Less than 300
10
300 or more
7.5
PRACTICAL LAB REPORT:AIM:THEORY:-
Calculations:-
Results of disintegration test: Time recorded for the capsules to break into particles and pass to the liquid medium = ---------------- minutes.
 Comment:
Results of weight variation test:

Average weight of the contents = (total wt. of the contents / 20) =

% deviation permitted (from the table) =

Upper limit (at % deviation)
= av. Wt. + (%/100 x av.wt.)
=

Lower limit (at % deviation)
= av. Wt. - (%/100 x av.wt.)
=

Upper limit (at double % deviation)
= av. Wt. + (double%/100 x av.wt.)
=

Lower limit (at double % deviation)
= av. Wt. - (double%/100 x av.wt.)
=
Caps.
No.
1
2
3
4
5
6
7
8
9
Wt. Of
intact
capsule
Wt. Of the
Wt. Of the
empty shell
content
Comparison Comparison
at %
deviation
at double %
deviation
10
11
12
13
14
15
16
17
18
19
20
Σ=
comment:
Suppositories
A suppository is a solid or semisolid mass intended to be inserted into a body orifice (e.g. the
rectum, Vagina, Urethra) to provide either a local or systemic therapeutic effect. Once inserted, a
suppository either melts at body temperature or dissolves (or disintegrates) into aqueous
secretions of the cavity.
Rectal suppositories are useful when oral administration is inappropriate, as with infants,
debilitated individuals, comatosed patients, and patients with nausea, vomiting and
gastrointestinal disturbances .Some drugs may cause irritation to the G.I.T. tract.
Preparation:Suppositories may be prepared by the following three methods:
I- Hand rolling involves molding the supp. With the fingers sifter the formation of a plastic mass
a.
A finely powdered drug is mixed with the grated
base in a mortar and pestle using livigation and
geometric dilution techniques .A small quantity
of fixed oil may be added to facilitate the preparation of
the mass.
b. The uniformly mixed semiplastic mass is kneaded
Further and then rolled into a cylinder.
II-Compression: is generally employed when cocoa butter
is used as a base.
III-The fusion method: is the principal way of making
suppositories commercially and is primarily used when
cocoa butter, PEG, an d glycerin-gelatin bases are used.
Examples:Method for determining displacement value
Using a nominal 2g mould:
Prepare and weigh six suppositories of un-medicated base = a gm .
Prepare base containing 30% medicament, fill six moulds and weigh six suppositories = b gm.
Calculate the amount of base c g, and the amount medicament d gm in the six suppositories
c = 70% b and d= 30 % b
Therefore tile amount of base displaced by
Dg = a – c gm
displacement value (D.V.) = d_
a-c
Example :
Weight of six unmediated suppos.
=6.0 g
30
% drug
Weight
of six suppos. Containing
Base = 70 % of 7.5
= 7.5 g
= 5.25
Drug = 30 % of 7.5
Base displaced by 2.25 g = 6 - 5.25
= 2.25
= 0.75 g
Therefore the displacement value of the drug = 2.25 = 3
0.75
Method for using displacement value
Required: to prepare for 8 suppositories each containing
300 mg drug of displacement value 3 using a normal 2 g mould.
Total amount of drugs required = 8 x 300 mg = 2.4 g
This will displace 2.4 = 0.8 g of base
3
Therefore amount of base required = 8- 0.8 = 7.2 g
Glycerin Suppositories
Gelatin dissolves in hot water, forming a solution which sets to a jelly. This fact is used to convert
glycerin into solid Corm for use as suppository. A suitable gelatin jelly is also used as a base for
other medicaments besides glycerin.
A gelatin base is incompatible with many of the substances prescribed in suppositories, e.g. tannic
acid, ferric chloride, gallic acid and for this and other reasons; it is less frequently used than cacao
butter. Glycerin suppositories containing ichthammol become insoluble on storage.
I. Glycerin Suppository B.P..
R/
Gelatin
Glycerin
Water QS to
14 g
70 g
100g
This is a suitable base for medicated suppositories containing solid medicaments or not
more than 20 per cent of semisolid or liquid medicaments. With more than this, the mass
becomes too soft.
Experiment – 11
Aim:- Preparation of glycerogelatin base suppositories
Rx
Gelatin
Glycerin
Water QS to
14 g
70 g
100g
Equipments Required:Mortar and pestle, Porcelain crucible, water-bath, 2 g x 6 mold
Chemicals:
Gelatin 84g, Glycerin 420 g, water 96 ml.
Procedure:
1.
Calculate for 6 supp., that is the amount of Gelatin = 6 x 14 = 84 g.
2.
Weigh the required amount of gelatin and soak it in enough water until thoroughly
softened.
3.
Put the soaked gelatin on the calculated amount of glycerin previously weighed
in a tared crucible and on a water bath until gelatin dissolves and a constant weight
is obtained.
4.
During evaporation the liquid mass should be only gently stirred, rapid stirring
produce air bubbles which may appear in the finished suppositories.
5.
Remove any skin formed on the surface before pouring.
6.
Pour the mass while still hot, into the holes lubricated with liquid paraffin, do not let the
melted mass to overflow.
Practical Lab Report
AIM:-
THEORY:-
Calculations:-
Observations & Results: