Pharmaceutics III, Department of Pharmaceutics
KINGDOM OF SAUDI ARABIA
UNIVERSITY PRINCE SATTAM BIN ABDULAZIZ
COLLEGE OF PHARMACY
LABORATORY MANUAL
PHARMACEUTICS III
PHT-322
LEVEL VI
Lab Co-ordinator
Dr. Shahid Jamil
Email:-
Contents
Page no / Remarks / Topics / Exp-No / Week
Powder and granules
Introduction / 1
Introduction / 2
Preparation of absorbable dusting powder / 1 / 3
Pulverization by Intervention / 2 / 4
Determination of angle of repose of given powders / 3 / 5
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. / 4 / 6
Determine the percent compressibility of 10 gm of magnesium sulphate powder by calculating the tapped and bulk density. Tabulate your results / 5 / 7
Send 20 gm of effervescent granules containing
20% of - Magnesium sulfate (Mg SO4), - Magnesium carbonate ( MgCO3 - or magnesium oxide (MgO) / 6 / 8
Send 20 gm of effervescent granules Sod. Citro-tartrate containing 25% of this mixture. / 7 / 9
Tablets
To prepare and compress 30 tablets each contains 0.9 g sodium chloride by direct compression method. / 8 / 10
To prepare and compress 20, tablets each contains sodium bicarbonate / 9 / 11
Capsule
Determination of the capsule fill weight / 10 / 12
Suppositories
To prepare six GlycerinSuppositoryB.P. / 11 / 13
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)
Powder and granules
Experiment 1
AIM: Preparation of absorbable dusting powder
Rx
Corn starch 98 g
Light magnesium oxide 2 g
Send 20 g
Sig.: to be used U.D.
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
Name of Experiment:
Date:
Student Name: ID#:
1.AIM:
2. Theory/Principle:
3. Equipments:
4. Materials:
5. Calculations:
6 .Observations & Results:
EXPERIMENT 2
AIM: Pulverization by Intervention
It is the reduction of particle size with the aid of a second agent which can be readily removed from the pulverized product
Procedure :
- Weigh 1g of camphor crystal
- It is readily triturated when a few drops of alcohol or other volatile solvent is added.
- The pulverized camphor is readily recovered as the solvent evaporates.
Practical Lab Report
Name of Experiment:
Date:
Student Name: ID#:
1.AIM:
2. Theory/Principle:
3. Equipments:
4. Materials:
5. Calculations:
6 .Observations & Results:
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
capsules.
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 flow able.
Factors affecting Powder Flow ability:
1- Particle size: -Frictional and cohesive forces (resistance to
flow.) are increased as the particle size is reduced
.
2- Density and porosity: -Particles with density and low porosity tend to posses free flowing properties.
3- Particle shape and surface texture:-Rough irregular particles presents more points of contact than smooth spherical particles and less free flowing.
4- Particle size distribution: - larger amount of fines can inhibit
poor Flowing.
5- Moisture: -Drying the powders will reduce the cohesiveness.
EXPERIMENT (3)
AIM:- DETERMINATION OF ANGLE OF REPOSE OF POWDERS
In this procedure we will measure the flow characteristic of some powders of pharmaceutical interest. And study the effect of glidents on the flow characteristics of various powders.
PROCEDURE:-
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 )
Tan the angle of repose ( Ø ) = h / r , get Ø , and tabulate your results.
Practical Lab Report
Name of Experiment:
Date:
Student Name: ID#:
1.AIM:
2. Theory/Principle:
3. Equipments:
4. Materials:
5. Calculations:
6 .Observations & Results:
Table (1)
Powder
/ Height (h) / Radius (r) / h/r / RemarkSodium chloride crystalline
Lactose2 % Talc
Sodium chloride crystalline + 2% Talc
Lactose + 2% Talc
Relationship between angle of repose and powder flow
Angle of Repose (θ) / Flow< 25 / Excellent
25–30 / Good
30–40 / Passable
> 40 / Poor
Density and Porosity of Powders
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 (%)
Example;A Sample of calcium oxide powder with a true density of 3.03 gm / cc and weighing 131 gm was found to have a bulk volume of 82.0 cc when placed in a 100 ml graduated cylinder. Calculate the porosity.
The volume of the particles is 131.3 gm / 3.203 gm / cc = 41. 0 cc
The volume of void space = 82.0 - 41 = 41 cc.
The porosity = 82-41 = 41 = 0.5 or 50 %
82
Problem (I)
Calculate the porosity of a sample of A having density of 4 gm/ cc when 75 gm of the powder was placed in graduated cylinder, the Awas found to have bulk volume of 62 cc.
Experiment (4)
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.
Practical Lab Report
Name of Experiment:
Date:
Student Name: ID#:
1.AIM:
2. Theory/Principle:
3. Equipments:
4. Materials:
5. Calculations:
6 .Observations & Results:
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 Ptand PBare the tapped and bulk densities respectively
Experiment (5)
Determine the percent compressibility of 10 gm of magnesium sulphate powder by calculating the tapped and bulk density.Tabulate your results
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.
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 chalkyfriable granules and citric acid is too sticky to be manipulated.It is desired thatcitric acid and tartaric acidare to be used in the ratio of 1:2respectively.
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 C02
c-The time required until effervescenceceases.
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 theresults 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 No:6
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 direct-flame 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
Name of Experiment:
Date:
Student Name: ID#:
1.AIM:
2. Theory/Principle:
3. Equipments:
4. Materials:
5. Calculations:
6. Observations:
Evaluation of the granules:
Quality control tests
Label :
Uses :
Magnesium sulfate granules:
7. Results:
Experiment No:7
Send 20 gm of effervescent granules Sod. Citrotartriate ot containing 25% of this mixture:
Rx
Zinc Oxide 10 gm
Starch Solution Qs
Fiat : (3%) Granules
Send 20-gm
Practical Lab Report
Name of Experiment:
Date:
Student Name: ID#:
1. Principle:
2. Equipment:
3. Materials:
4. Calculations:
5.Observations:
Quality control tests
6.Label and Uses:
7.Results:
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 theprinciple 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
Acompressed tableis a unitdosageform_preparedby compressing medicinalsubstanceinapowderorgranular 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:
Theseare substances inert and stable used to increase the
volumeofthetablet.
Soluble: eg Lactose, sucrose,mannitotsorbitoL
Insoluble:eg Calcium sulfate, dicalcium phosphate ,
tricalcium phosphate starch calcium carbonate .
2- Binders or Adhesives-
Theseare 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
- Acacia mucilage 10-20%
-Tragacanth mucilage 10-20%
- Gelatin solutions / 3-10%- Starch mucilage / 5-10%
- Glucose syrup / 25-50%-67%
Cellulose derivatives / 3-10%
3- Disintegratents:
Thesearematerialsthathelptabletbreakupintosmall particles in the gastrointestinal tract.
Examples :
Starch, alginates, cellulose derivatives, and lactose
Disintegratesadded 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 areagentsthat reduce the frictionbetween 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,stearicacid, talc.
6-Glidantsare Materialsthat improve the flow characteristics of
granulation. Example:- Talc
7-Anti- adherents:
Are materials usedto prevent tablet sticking to the faces of ft punches and die walls.Example: Talc.
8- Other table components
These arecoloring 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 uniformfill of the die cavity.
Experiment No:8
Direct Compression:
1-Sodium chloride tablets
Aim: To prepare and compress 30 tablets each contains 0.9 g sodium chlorideby direct compression method
.
Rx
Sodium chloride 0.9 g
Notes for preparation:
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
Name of Experiment:
Date:
Student Name: ID#:
1. Principle:
2. Equipments:
3. Materials:
4. Calculations:
5 .Observations & Results:
Description:
Label:
Uses
Tablets used in preparation of isotonic solutions
One tablet dissolved in sufficient water for injection and the volume completed to 100 ml.
Storage: