PD-403 PHARMACEUTICS-IVB (INDUSTRIAL

PHARMACY) LAB MANUAL

Name: ___________________________________
Registration No: ___________________________
Semester: ________________________________
Section: ________________________________

MUHAMMAD HARIS JALAL

LECTURER DEPAERTMENT OF PHARMACY | ABASYN UNIVERSITY
ISLAMABAD CAMPUS
 CERTIFICATE

This is certified that ____________________________________ enrolled with

Registration number _____________________of Pharm-D 8th Semester, spring
2024 has satisfactorily carried out all the practical activities regarding the Course
code PD-403 Pharmaceutics-IVB (Industrial Pharmacy).

Student Signature: _________________________________________

Lab Instructor: _______________________________________________

Concerned Teacher: __________________________________________

External Examiner: __________________________________________

 INDEX

S.NO EXPERIMENT DATE SIGNATURE

S.NO EXPERIMENT DATE SIGNATURE
 EXPERIMENT: 01

AIM: To perform different preformulation studies of prepared granules.

REQUIREMENTS: Measuring Cylinder, Funnel, Sieves, Mortar & Pestle, Spatula.

PRINCIPLE: Preformulation is defined as the phase of research and development in which
preformulation studies characterize physical and chemical properties of a drug molecule in order
to develop safe, effective and stable dosage form. The Objective of preformulation study is to
develop the elegant, stable, effective and safe dosage form by establishing kinetic rate profile,
compatibility with the other ingredients and establish Physico-chemical parameter of new drug
substances. The major preformulation studies/parameters of granules are as follows:

1. Bulk density: It is defined as ratio of total mass of the powder to the bulk volume of powder.
It gives an idea about tablet porosity and its relationship with disintegration time and hardness
of a tablet. It is measured by pouring weighed powder into a measuring cylinder and the volume
is noted down. It is expressed in gm/ml and is given by
Db=M/Vo
Where, M= Mass of powder, Vo = Bulk volume of powder.
2. Tapped density: It is defined as ratio of total mass of the powder to the tapped volume of
powder. Tapped volume is measured by tapping the powder to constant volume. It is expressed
in gm/ml and is given by:
Dt=M/Vt
Where, M= Mass of powder, Vt = Tapped volume of powder
3. Angle of repose (Ɵ): It is the maximum angle possible between surface of pile of powder and
the horizontal plane, can be used to measure frictional forces in a powder.
Ɵ= tan-1 (h/r)
Where, Ɵ= angle of repose H height of the powder in cm, R is the radius of heap of powder.

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Relationship between Angle of reposes and flow property
Angle of repose Flow property
5-15 Excellent
12-15 Good
15-22 Fair
23-30 Poor
33-38 Very poor
>40 Extremely poor

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 VIVA-VOCE QUESTIONS

1) What is the significance of preformulation studies in pharmaceutical development?

2) What is the significance of preformulation studies in pharmaceutical development?

3) What is the significance of preformulation studies in pharmaceutical development?

4) Briefly discuss the pharmaceutical applications of Angle of Repose?

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 EXPERIMENT: 02

FILLING OF HARD GELATIN CAPSULES USING MANUAL OPERATION

CAPSULES FILLING MACHINE

1. Requirements
• Capsule filling machine
• Empty hard gelatin capsules
• Powder to be filled into capsules

2. Procedure
1. Place empty capsules onto the loading tray and place tray onto the machine. Check the
knob on the left side, it should be turned to the right (to lock the loading tray).
2. Pull locking lever forward (toward the operator).
3. Move out the left knob in the outward direction (to open the loading tray).
4. Push down long handle called lifting lever which will lifts the caps off all the bodies. Set
aside the tray containing all the caps.
5. Push locking lever back, by which capsule bodies will drop down and become level with
filling surface.
6. Place powder tray on filler: keeps powder from spilling.
7. Pour & spread the pre-measured powder. Move extra powder onto powder tray's shelf.
Lower tamper and lock.
8. Turn handle to compress powder: this allows you to fill more powder in each capsule.
9. Raise tamper & spread extra powder from shelf into capsules: ensures uniform fill weights.
10. Return the tray containing caps to filler. Lower locking plate. Engage lock for locking plate.
11. Push the left knob to the right. Hold tamper handle and push down on long handle (lifting
lever). Bodies are pushed up into caps: all the capsules are now locked in one step.
12. Disengage lock for locking plate. Lift locking plate and turn left knob to the left side.
13. Push down long handle (lifting lever) and remove tray of completed capsules.
14. Capsules are filled now. You can turn tray and all the capsules will get out from the tray.

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 VIVA-VOCE QUESTIONS

1) Describe the basic operation of a manual capsule filling machine?

2) What are the advantages and limitations of using a manual capsule filling machine
compared to automated machines?

3) How do you ensure uniformity and accuracy in filling hard gelatin capsules using a
manual machine?

4) What are the critical parameters to consider during the filling process to maintain product
quality and consistency?

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 EXPERIMENT NO 03

TO REDUCE THE PARTICLE SIZE OF POWDER USING BALL MILL

Ball milling is a method used to break down the solids to smaller sizes or into a powder. A ball
mill is a type of grinder which consists of a cylinder. The cylinder rotates around a horizontal axis.
It is partially filled with the grinding medium and the material to be ground. Materials which can
be used as media are ceramic balls, pebbles and stainless-steel balls.

Requirements
• Sieve set
• Coarse powder
• Ball mill and steel balls
• Stainless steel container

Procedure
1. Weigh the 1-2 kg of coarse powder.
2. Add the coarse powder into the sieve arranged in such order that sieve with bigger pore
size should be at the top of the sieve set followed by sieve with smaller one
3. Shake the sieve set using sieve shaker for 8 minutes.
4. Calculate the weight fraction for amount of powder retained on each sieve by formula:
Weight reatained on the sieve
5. Weight fraction = total weight of the powder

6. Plot the graph of particle size distribution using Microsoft Excel.

7. Insert steel balls of known sizes into the ‘mill’.
8. Add the coarse powder into the ‘mill’.
9. Turn the ball mill so that it starts rotating its own axis and rotate it for 10 or 20 minutes
with the appropriate speed.
10. Collect the product in container.
11. Sieve again the powder obtained using sieve shaker.
12. Plot the graph of particle size distribution using Microsoft Excel.
13. Compare the particle size distribution of powder before milling and after milling.

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 VIVA-VOCE QUESTIONS

1) Can you explain the principle of operation of a ball mill for particle size reduction?

2) How does the speed and rotation direction of the ball mill affect the particle size
reduction process?

3) Discuss the types of milling media used in a ball mill and their impact on particle size
reduction.

4) What factors influence the efficiency of particle size reduction in a ball mill?

5) How do you evaluate the particle size distribution and uniformity of the milled powder?

6) Compare and contrast the advantages and limitations of ball milling with other methods
of particle size reduction

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 EXPERIMENT NO 04

PREPARATION OF SYRUP (B.P) USING SILVERSON MIXER

Requirements
Sugar 667 gm
Water Q.S to produce 1000 gm
Equipments
Weighing Balance
Silverson Mixer

Procedure
1. Take water in the container
2. Star the mixer.
3. Add the sugar portion wise into the water present in the Silverson Mixer.
4. The high shear action of the mixer rapidly breaks down the sugar granules exposing
the largest possible surface area of sugar to the water which will greatly accelerates
the solubilization process.
5. Mix it until all the sugar dissolves.

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 VIVA-VOCE QUESTIONS

1) Discuss any challenges or limitations associated with using a Silverson mixer for syrup
preparation, and how they can be addressed.

2) What measures are taken to ensure uniformity and consistency in the syrup formulation
during mixing with a Silverson mixer?

3) What are the critical parameters to monitor during syrup preparation using a Silverson mixer,
and how are they controlled?

4) How do you validate the mixing process and ensure that the final syrup meets the required
quality standards?

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 EXPERIMENT NO: 05

PREPARATION OF PARACETAMOL GRANULES BY WET GRANULATION USING

OSCILLATING GRANULATOR

Introduction

Wet granulation is the process of tablet formation in which we make the wet mass by adding
binding agent in the solution to form the granules of the powder. Lubricant is added at the last
stage. Wet granulation is the process of formation of tablet that is used for those tablets that are
the heat and moisture resistant.

Equipments

• Weighing Balance
• Oscillating Granulator
• Tray Dryer

Chemicals

For 1 tablet For 500 tablets Role

Chemical Name

Paracetamol 500 mg 250 mg API

PVP k30 (Polyvinyl 25 mg 12.5 Binder
pyrrolidone)
Starch 35 mg 17.5 Disintegrant
Procedure
1. Mix the paracetamol and starch for 20 minutes using double cone mixer.
2. Add the accurately weighed quantity (12.5gm) of binder PVP k30 (Polyvinyl pyrrolidone) to
250ml of distilled water with continuous stirring and heat it until a clear solution is obtained.
3. Add the binder to the powder by spreading all over the powder and knead it for 20 minutes to
obtain damp mass.
4. Pass the damp mass through oscillating granulator and dry it in tray drier at 60 ºC for 1 hour.

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 VIVA-VOCE QUESTIONS

1) What measures are taken to evaluate the quality of paracetamol granules prepared by wet
granulation, and how do you ensure uniformity and consistency in the final product?

2) What are the critical parameters to monitor during wet granulation with an oscillating
granulator, and how are they controlled?

3) Explain the role of water in the wet granulation process and how it affects the granulation
outcome.

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 EXPERIMENT NO: 06
FILLING, CAPPING AND SEALING OF SYRUPS BOTTLES

Introduction:

Syrup bottle filling machine is made compact, versatile and enclosed in stainless steel elegantly
matt finish body. This unit works on volumetric principal

Syrup capping machine is a device that tightly packed the container to exclude oxygen, carbon
dioxide, moisture, and microorganism and prevent loss of water and volatile substance from
products during transport and handling.

Requirements:

➢ Syrup
➢ Syrup bottles
➢ Caps
➢ Syrup filling machine
➢ Syrup capping machine

Procedure:

1. Check that syrup filling machine is cleaned properly. If not satisfactory, clean it.
2. Syrup is placed in syrup manufacturing tank
3. Take bottles of either volume of 90ml or 60ml.
4. Clean the bottle thoroughly.
5. Adjust the volume to be filled in bottle of the machine.
6. Now dip the pipe of machines into the syrup manufacturing tank.
7. Place the bottles beneath the nozzle of machine.
8. Switch ON the machine.
9. Fill the bottles and check for volume by measuring cylinder if correct volume is filled or
not.
10. After filling, capping of bottles is done by syrup capping machine.
11. Keep the cap on the bottle and keep the bottle under the roller head on the base plate.
12. Switch ON the machine and thread the cap with sealing rollers by lifting the base plate.

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13. After sealing of the cap of the bottle, replace it with another bottle and continue the process.
14. After completion of the sealing operation, clean both machines.
15. Wash all the parts with tap water and clean it with dry cloth

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 VIVA-VOCE QUESTIONS

1) What are the regulatory requirements and quality control measures associated with the
filling, capping, and sealing of syrup bottles in pharmaceutical manufacturing?

2) What measures are taken to prevent contamination during the filling, capping, and sealing
process?

3) Discuss the different types of capping machines used for sealing syrup bottles and their
respective advantages.

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 EXPERIMENT NO: 07

FILLING OF DRY SUSPENSION ON POWDER FILLING MACHINE

Powder filling machine ensures uniformity in the filling process to produce more precise powder
fills.

Requirements:

➢ Powder to be filled
➢ Powder Filling Machine

Procedure:

1. First of all, make sure the powder filling machine is clean and working properly.
2. Accurately weigh the amount of powder that is to be used.
3. Now turn ON the machine.
4. The operator supplies bulk amounts of the powder product into the hopper and feeds the
machine with empty containers.
5. The conveyor directs the empty containers and positions them below the filling head.
6. The machine measures/weighs the powder product to be dispense into each container.
7. The filling head dispenses consistent amounts of the powder product into each container.
8. After the whole process is done, turn OFF the machine.
9. Make sure to properly clean the machine after operation.

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 VIVA-VOCE QUESTIONS

1) How are filled containers inspected to ensure they meet quality standards before
packaging?

2) What are the regulatory requirements and quality control measures associated with
filling of suspension?

3) Describe the basic principle of operation of a powder filling machine for filling dry
suspensions?

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 EXPERIMENT NO: 08
PREPARATION OF PARACETAMOL TABLETS BY WET GRANULATION
USING SINGLE PUNCH MACHINE

Introduction

Wet granulation is the process of tablet formation in which we make the wet mass by adding
binding agent in the solution to form the granules of the powder. Lubricant is added at the last
stage. Wet granulation is the process of formation of tablet that is used for those tablets that are
the heat and moisture resistant.

Equipments
• Weighing Balance
• Oscillating Granulator
• Tray Dryer
• Single punch machine
Chemicals

Chemical Name For 1 tablet For 500 tablets Role

Paracetamol 500 mg 250 gm API

PVP k30 (Polyvinyl pyrrolidone) 25 mg 12.5 gm Binder
Starch 35 mg 17.5 gm Disintegrant
Magnesium stearate 100 mg 50 gm Lubricant

Procedure

Pass the paracetamol and starch through sieve no 16 and mix for 20 minutes using double cone
mixer.

Add the accurately weighed quantity of binder to distilled water with continuous stirring and heat
it until a clear solution is obtained.

Add the binder to the powder by spreading all over the powder and knead it for 20 minutes to
obtain damp mass.

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Pass the damp mass through oscillating granulator and dry it in tray drier at 60 ºC for 1 hour.
When granules formed, add accurately weighed quantity of lubricant (magnesium stearate)
After that tablets are formed using single punch machine.

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 EXPERIMENT NO: 09

PREPARATION AND FILLING OF OINTMENT

Introduction:

An ointment is a semi solid preparation of a medication for topical use that contains an oil base -
essentially a preparation of water in oil or without using water.

Equipment:

Weighing balance, hot plate, water bath, ointment filling machine

Raw Materials:
Wool fat (lanoline), Hard paraffin, Cetostearyl alcohol, White soft paraffin

Material Quantity [for 1000g]

Wool fat (lanoline) 50 g

Hard paraffin 50 g
Cetostearyl alcohol 50 g
White soft paraffin 850 g

Procedure:

1. Heat wool fat, hard paraffin and cetostearyl alcohol to melt at about 65 C.

2. Heat white soft paraffin at about 70 C and continuously stir until at room temperature

3. When the product is ready, transfer it to the filling machine

4. Add it to the hopper of ointment filling machine.

5. Place ointment tube at the nozzle of ejecting oitnment.

6. Start the machine after adjusting the mass of ointment to be filled.

7. Remove the filled ointment & replace by empty.

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 EXPERIMENT NO: 10

PREPARATION OF COD LIVER OIL EMULSION USING PROPELLER MIXER

Requirements

Cod Liver Oil 25 ml

Acacia 10 g

Double Strength Chloroform Water 250 ml

Freshly boiled and cooled purified water to 500 ml

Preparation of double strength chloroform water:

Add 5 ml chloroform to quantity sufficient purified water to produce 100 ml.

Procedure:

1) Transfer the 25 ml of Cod Liver Oil to a clean dry porcelain mortar.

2) Transfer the 5g Acacia to the mortar and stir gently
3) Add the 30 ml of Double Strength Chloroform Water to the mortar in one go.
4) Stir vigorously with the pestle in one direction only until the primary emulsion is formed.
5) Add more Double Strength Chloroform Water to the primary emulsion until the emulsion
is pourable.
6) Transfer to an appropriate conical measure with rinsing.
7) Make up to volume with any remaining Double Strength Chloroform Water and freshly
boiled and cooled purified water and stir it with Propeller mixer.

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 EXPERIMENT NO: 11

FORMULATION OF FILM COATED TABLETS OF PARACETAMOL

AIM: To prepare 10 tablets of paracetamol film coated tablets.

REQUIREMENTS: Mortar and pestle, Sieve, Beaker, Glass rod

PRINCIPLE: All drugs have their own characteristic, like some drugs are bitter in taste or have

an unpleasant odor, some are sensitive to light or oxides, some are hygroscopic in nature. Because

of this reasons, tablet coating is the choice of option to solve such problems in conventional dosage

form. Tablet film coating is performed by two types, one is aqueous film coating (generally water

is used as a solvent) and non-aqueous film coating (generally organic solvents are used). Some

problems are associated with the non-aqueous film coating like safety of employees (as most of

the solvents are dangerous, smell, and they are not good to breathe), atmospheric pollution etc. But

key problem is with the approval of the regulatory authority. High quality aqueous film coating

must be smooth, uniform and adhere satisfactorily to the tablet surface and ensure chemical

stability of a drug. Coating may be applied to a wide range of oral solid dosage forms, including

tablets, capsules, and multiparticulate and drug crystals. When coating composition is applied to a

batch of tablets in a coating pan, the tablet surfaces become covered with a tacky polymeric film.

Before the tablet surface dries, the applied coating changes from a sticky liquid to tacky semisolid

and eventually to a non-stick dry surface. The entire coating process is conducted in a series of

mechanically operated acorn-shaped coating pans of galvanized iron stainless steel or copper. The

smaller pans are used for experimental, developmental, and pilot plant operations, while the larger

pans for industrial production.

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Necessity of Tablet Coating:

• A number of reasons can be suggested, like: The core contains a material which has a bitter

taste in the mouth or has an unpleasant odour. Coating will protect the drug from the

surroundings with a view to improve its stability.

• Coating will increase the ease by which a tablet can be ingested by the patient.

• Coating will develop the mechanical integrity; means coated products are more resistant to

mishandling (abrasion, attrition, etc.)

• The core contains a substance which is incompatible in the presence of light and subject to

atmospheric oxidation, i.e. a coating is added to improve stability.

• The coated tablets are packed on high-speed packaging machine. Coating reduces friction

and increases packaging rate.

• Coating can modify the drug release profile, e.g., enteric coating, osmotic pump, pulsatile

delivery

Formula:

Name of ingredients Quantity (% W/W)

Cellulose acetate 6.3
PEG-400 0.7
Acetone 89
Deionized water 4

PROCEDURE: Paracetamol uncoated tablets are prepared by wet granulation method. The
prepared tablets are then coated with film coating solution prepared as below.

FILM COATING SOLUTION PREPARATION: The coating solution was prepared by

dissolving PEG in water followed by addition of this solution to acetone. Cellulose acetate was
then added to the above mixture and stirred to achieve a clear solution. The coating process was

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performed in a Vector Hi-Coater LDCS (batch size, 1.5 kg, with inclusion of placebo tablets) at a
product temperature of 28ºC. Coated tablets were dried in a vacuum drying oven at 40ºC for 24
hours to remove residual solvent and moisture.

REPORT: 10 tablets of paracetamol film coated tablets are prepared and submitted.

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 EXPERIMENT NO: 12

PREPARATION OF ASCORBIC ACID INJECTION

AIM: To prepare and submit 2 ml ascorbic acid injection.

REQUIREMENTS: Beaker, Glass rod, Funnel, Filter paper, Ampoule

PRINCIPLE:

Injections are sterile solutions, emulsions or suspensions. They are prepared by dissolving,
emulsifying or suspending an active ingredient and any other substances in water for injection.
Injecting is the act of giving medication by use of syringe and needle to obtain the desired
therapeutic effect taking into account the patient’s safety and comfort. It is suitable for those drugs
that are altered or not absorbed by other methods of administration. Ascorbic Acid (vitamin C) is
a water-soluble vitamin. It occurs as a white or slightly yellow crystal or powder with a light acidic
taste. It is an antiscorbutic product. Ascorbic Acid injection is a clear, colourless to slightly yellow
sterile solution of Ascorbic Acid in Water for Injection, for intravenous, intramuscular or
subcutaneous use.

Formula:

Ingreients 1 ampoule 2 ampoule

Ascorbic acids 0.5 gm 1 gm
Water for injection 2 ml 4 ml

PROCEDURE: Ascorbic acid is dissolved in water for injection in a beaker and makes upto
required volume. Filter it and take 2 ml of the filtrate. Then it is transferred into previously
sterilized ampoules, sealed properly and sterilized by autoclaving.

USE: It is used as anti-scurvy.

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 EXPERIMENT NO: 13

FORMULATION OF ENTERIC COATED TABLETS OF OMEPRAZOLE

AIM: To prepare 10 tablets of enteric coated tablets of omeprazole.

REQUIREMENTS: Mortar and pestle, Beaker, Sieve, Glass rod

PRINCIPLE: Enteric coatings are primarily used for the purpose of:

• Maintaining the stability of APIs that are unstable when exposed to the acidic conditions

of the gastric milieu. Such API’s include erythromycin, pancreatic, and the class of

proton pump inhibitors, such as omeprazole.

• Minimizing the side effects (eg, nausea, and gastric irritation and bleeding) that can occur

with APIs such aspirin and certain nonsteroidal inflammatory compounds.

• Creating opportunities for “night-time dosing” strategies, where the intent is to allow the

dosage form to be consumed at bed-time, and permit effective blood levels of the API to

be attained just prior to waking.

• Facilitating colonic drug delivery. The functionality of enteric coatings is, for the most

part, mediated by a change in pH of the environment to which the enteric-coated product

is exposed. Enteric polymers remain unionized (and thus, insoluble) at low pH values,

and begin to dissolve at a pH value of approximately 5.0–5.5.

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PROCEDURE:

WET GRANULATION:

• Weigh accurately require quantity of Omeprazole, Lactose , Sodium starch glycolate ,

Sodium Lauryl Sulfate, Magnesium hydroxide and pass through sieve no #40

• Prepare a binding solution by dissolving HPC in water and stir binder solution for 10

minutes, this solution is added to dry mix to form granules.

• The prepared granules are dried and lubricated with lubricants.

• The lubricated granules are then compressed to form immediate release tablets.

Seal Coating: Prepare sub coating solution using HPMC or PVA in Purified water. Coat the

uncoated tablets with the seal coating suspension to achieve required weight gain.

Enteric coating: Prepare enteric coating suspension using HPMC Phthalate, Triacetin, and Talc

in Acetone-IPA mixture. Coat the uncoated tablets with the enteric coating suspension to achieve

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required weight gain.

REPORT: 10 tablets of omeprazole enteric coated tablets are prepared and submitted.

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