LAB REPORT
Course Title: Pharmaceutical Technology III Lab
Course Code: PHAR 3206
Contents
Experiment No | Name of the experiments | Page no | Date |
1 | Weight variation test of tablets. | 2-4 | 5-11-2023 |
2 | Friability test of tablets. | 5-7 | 5-11-2023 |
3 | Determination of disintegration time of tablets | 8-11 | 5-11-2023 |
4 | Preparation and formulation of paracetamol tablets. | 12-13 | 5-11-2023 |
5 | Preparation of whit-field Ointment. | 14-17 | 5-11-2023 |
Experiment No: 01
Name of the Experiment: Weight variation test of tablets.
Principle:
Weight variation test is the test by variation of weight from tablet to tablet determined. The following formula is which can be used,
Weight variation= Iw-Aw Aw × 100%
Iw = Individual weight of tablet
Aw = Average weight of a tablet
The acceptable range according to USP:
Due to a variety of reasons, excessively overweight on tablets may be problematic. To alleviate this problem the United States Pharmacopoeia (USP) / National Formulary (NF) provides limits for the permissible variation of weight of individual tablets expressed as a percentage of the average weight of sample. The USP weight variation test is run by weighing 20 tablets individually, calculating the average weights and comparing the individual tablet weights to the average.
The tablets meet the USP test, if not more than 2 tablets are outside the percentage limit, and if no tablet differs by more than two times of the percentage limit. The weight variation tolerance for uncoated tablets differs depending on the average tablet weight.
Weight Variation Tolerance for Uncoated tablets
Average wt. of tablet (mg) | Maximum Percentage Difference Allowed |
130 or less | 10% |
130-324 | 7.5% |
More than 324 | 5% |
Why is weight variation test done?
The weight of tablet is the quantity of granules which contain the label amount of the therapeutic ingredients. The volumetric fill of the die cavity determines the weight of the compressed tablet. In setting up, the tablet machine is operated. The weight of the tablets are checked routinely either manually or electronically, to ensure proper weight of tablets which are being made.
A large weight variation precludes good content and uniformity. The patient receiving the tablet may be overdosed or under dosed due to weight variation.
Some possible reasons for weight variation:
Erratic punch flight
Material loss due to lack of proper die fills.
Feeder "starved" or "choked"
Die not filling
Lower punch starts pulling
Bad scrubs-off
Supplied Sample:
Generic Name: Paracetamol 500 mg
Procedure:
Each of the 6 tablets is weighted separately by using an electronic balance.
All of the 6 tablets are weighted and the average weight is calculated.
Weight variation of each tablet is calculated individually by using the formula.
Data:
Tablet Number | Individual weight Iw (mg) | Average weight Aw (gm) | Weight Variation= Iw-Aw Aw × 100% |
1 | 538.1 |
| 4.390% |
2 | 511.5 |
| -0.770% |
3 | 495.3 | 515.47 | -3.913% |
4 | 509.4 |
| -1.178% |
5 | 522.0 |
| 1.267% |
6 | 516.5 |
| 0.199% |
Comments:
All the tablets were within the range of weight variation according to USP.
Precautions:
1. All the instruments were cleaned and handled carefully.
2. Apron was worn in the laboratory.
3. Volume was measured cautiously.
Experiment No: 02
Name of the Experiment: Friability test of tablets.
Principle:
Friability of tablet is defined as the capacity of tablet to withstand shock and abrasion during packing, handling, and shipping. It is determined by the following formula:
Friability = Iw-Fw lw × 100%
Iw = Initial weight of tablets
Fw = Final weight of tablets
Acceptable range according to USP:
Conventional compressed tablets lose weight less than 0.5% to 1% (After 100 revolutions) of their initial weight. The rang is generally considered acceptable.
Why is the friability test done?
The friability test is done due to the following reasons:
Friable tablets no longer have a sharp edge. Consequently, pharmaceutical elegance and patient acceptance is diminished.
Tablet friability results in weight loss of tablets owing to partial chipping or fragmented.
Weight loss due to excessive friability may affect therapeutic response.
Description of the Friability Test Machine:
Tablet friability is related to tablet hardness and the measurement is made by use of a friabilator rather than the force required to crush the tablet. An instrument is designed to evaluate the ability of the tablet to withstand abrasion during packing, handling, and shipping.
The device has two circular chambers which rotate at 30 rpm, the tablets are dropping at a distance of 6 inches with each revolution when machine is operated. A device facilitates time setting. There is no option of revolution setting and the machine stops automatically.
A number of tablets are weighed and placed in the tumbling apparatus where they are exposed to rolling and repeated shock. Then tablets are taken from the machine and weighed again and loss in weight indicates friability of the tablet.
Supplied Sample:
Generic Name: Paracetamol 500 mg
Procedure:
Each of the 6 tablets is weighed separately by using an electronic balance.
The friabilator is then set for 5 min with 150 revolutions and all the tablets placed in the apparatus and it is turned on.
During this period, the tablets are exposed to rolling and repeated shocks resulting from free falling within the apparatus.
When the device stops, the tablets are automatically collected and weighed again.
Result:
Initial wt. of all (6) tablets (Iw) = 6.7709 mg
Final wt. of all (6) tablets (Fw) = 6.7608 mg
Friability = Iw-Fw lw × 100%
= 6.7709 mg - 6.7608 mg6.7709 × 100%
= 0.01016.7709 × 100%
= 0.14916 %
Comments:
Conventional compressed tablets that lose less than 0.5-1% of their weight is generally considered as acceptable.
Precautions:
All the instruments were cleaned and handled carefully
Apron was worn in the laboratory
Volume was measured cautiously
Experiment No: 03
Name of the Experiment: Determination of disintegration time of tablet.
Principle:
Before absorption of a tablet takes place in the body, it must be in solution. For most tablets, the first important step toward a solution is the breakdown of the tablet into smaller particles or granules, this process known as disintegration. The time that takes the tablet to disintegrate is measured in a device which is described in the USP/NF.
Factors affecting disintegration:
If tablet's hardness is too high, this can be reduced by reducing machine pressure for acceptable range.
Over lubrication, this can also cause waterproofing. This can be reduced by blending lubricant only 5-10 minutes in the final mix and replacing metallic steerages with stearic acid.
Lack of disintegration agent.
pH of the medium such as in gastric fluid, and intestinal fluid.
Description of the Machine:
The USP device, to test disintegration, uses six glass tubes that are 3 inches long, open at the top and held against a 10-mesh screen at the bottom end of the basket rack assembly.
Procedure:
To test for disintegration time on paracetamol 500 mg tablet is placed in each tube and the basket rack positioned in a 1L beaker of water at 37°C, such that the tablets remain 2.5 cm below the surface of the liquid, their upward movement and descent not closer than 2.5 cm from the bottom of the beaker.
A standard motor-driven device is used to move the basket assembly, then the tablets move up and down through a distance of 5 to 6 cm at a frequency of 28 to 32 cycles/min.
Perforated plastic discs may also be used in the test. These are placed on the top of tablets and impart an abrasive action to the tablets.
The discs may not be meaningful or impart more sensitively to the test, but are useful for tablets that float.
To create a basic media, we used a 0.1N NaOH solution.
Disintegration time for paracetamol 500 mg tablets as mentioned in USP we found that:
Tablet Number | Disintegration Time |
1 | 64 sec |
2 | 66 sec |
3 | 69 sec |
4 | 72 sec |
5 | 68 sec |
6 | 75 sec |
Comments:
To comply with the USP standards, the tablets must disintegrate, and all particles must pass through the 10-mesh screen in the time specified.
If any residue remains, it must have a soft mass with no palpably firm core. Uncoated tablets have disintegration time standards as low as 5 minutes.
Majority of the tablets have maximum disintegration after a time of 30 minutes.
Enteric coated tablets show no evidence of disintegration after 1 hour in simulated gastric fluid.
The same tablets are then tested in stimulated intestinal fluid and are to disintegrate in 2 hours.
Explanation:
The value of the result of paracetamol 500 mg tablets has a disintegration time which meets the USP standard which means disintegration into small particles and releases the drug before absorption could take place.
Material and Solutions:
Water (Use distilled water), Hydrochloric and (ACS reagent grade)
Sodium chloride (ACS reagent grade)
Pepsin (FCC grade), Potassium Phosphate, Monobasic (ACS reagent grade)
Pancreatin (USP grade)
Precautions:
All the instruments were cleaned and handled carefully.
Apron was worn in the laboratory.
Volume was measured cautiously.
Experiment No: 04
Name of the Experiment: Preparation and formulation of paracetamol tablets.
Principle:
A tablet (also known as a pill) is a pharmaceutical oral dosage form (oral solid dosage, or OSD) or solid unit dosage form. Tablets may be defined as the solid unit dosage form of medication with suitable excipients. It comprises a mixture of active substances and excipients, usually in powder form, that are pressed or compacted into a solid dose. The main advantages of tablets are to ensure a consistent dose of medication that is easy to consume.
Paracetamol is a widely used analgesic and antipyretic drug. It is used to treat mild to moderate pain and fever. Paracetamol is available in different dosage forms such as tablets, capsules, syrups, and injections
Apparatus:
Mortar & Pestle.
Electronic Balance.
Spatula.
Formulation: for 40 tablets
Ingredients | Amount |
Paracetamol Powder | 2000 mg |
Lactose | 800 mg |
Mg Stearate | 100 mg |
MC | 3000 mg |
Talcum Powder | 150 mg |
Acacia | 500 mg |
CaCO3 | 500 mg |
Procedure:
Preparation of ingredients: Weigh all the ingredients according to the desired dosage strength of the tablets. The ingredients include paracetamol (active ingredient), microcrystalline cellulose (binder), starch (disintegrant), and magnesium stearate (lubricant).
Mixing of ingredients: Thoroughly mix the ingredients in a blender for 10-15 minutes to form a homogeneous mixture. The blending time may vary depending on the amount of ingredients and the type of blender used.
Setting up the tablet machine: Ensure that the tablet machine is clean and properly assembled. Install the appropriate size and shape of the punch and die set for the desired tablet size and shape.
Loading the mixture: Load the homogeneous mixture into the hopper of the tablet machine. The hopper should be filled to the appropriate level, ensuring that the mixture is evenly distributed.
Compression of the tablets: Start the tablet machine and adjust the speed and compression force according to the desired tablet hardness and weight. The machine compresses the mixture into tablets by applying pressure from the upper and lower punches. The compressed tablets are then ejected from the machine.
Comments:
All the tablets were within the range of weight variation according to USP.
Precautions:
All the instruments were cleaned and handled carefully.
Apron was worn in the laboratory.
Volume was measured cautiously.
Experiment No: 05
Name of the Experiment: Preparation of whit-field Ointment.
Principle: Ointments are the soft semi-solid preparation meant for external application to the skin or mucous membrane. They usually contain a medicament that dissolved, suspended on emulsified base. Ointments are used for emollient and protective action to the skin.
The ointment of benzoic acid or salicylic and is called whit-field ointment. It contains benzoic acid and salicylic acid in ratio of a 2:1 (usually 6% : 3%)
Advantages of ointments are, it melts at body temperature and easily applied to the skin, gives very smooth and soothing effects, it also has long period of contact with skin. One disadvantages of ointment is that it can't be easily removed from the skin because it contains oily substances.
Ideal properties of Ointments:
It should be chemically and physically stable.
It should be smooth and free from grittiness.
It should melt or soften at body temperature and be easily applied.
The base should be non-irritating and should have no therapeutic action.
The medicament should be finely divided and uniformly distributed through the base.
According to therapeutic uses ointments are various types:
Anti-eczematous
Antibiotic
Antifungal
Counter irritant
Keratolytic
Anti-inflammatory
Antipruritic
Astringent
Emollient
Various ointment bases are used in ointment preparation. These are:
Apparatus:
Electronic Balance
Spatula
Dropper
Mortar and pestle
Beaker
Stirrer
Water bath
Test Tube
Reagents:
ΑΡΙ
Excipients
Distilled water
Formulation
Ingredients |
Purpose
| Amount (gm) |
Salicylic acid (3%)
| Active ingredient | 0.75 |
Benzoic Acid (6%) | Active ingredient | 1.5 |
Paraffin Base (Vaseline)
| Ointment base Raising melting Point
| Q.S. to 25 |
Hard Paraffin
| Stiffening agent Increases viscosity
| 1.2 |
Soft Paraffin | | 2.5 |
Procedure
Petroleum jelly (Vaseline) and soft-paraffin were taken in a mortar and triturated gently using little amount of water.
Hard paraffin was added with triturating.
The content was taken in a beaker, it was heated to melt. The temperature should be above 50°C and below 80°C. Water bath was set to 80°C.
The base was cooled at 50-60°C and the active ingredients (benzoic and salicylic acid) were added.
The ointment was cooled down to normal temperature.
Then it was parked in a labeled container.
Labelling
Whit-field Ointment 25 gm Each gram contains Salicylic acid 0.3 gm & Benzoic acid 0.6 gm Uses: Topically, Ringworm / Teneasis, Eczema etc Mfg Date: 5-11-2023 Exp Date: 5-11-2023 Batch No: 01 Manufactured By X Pharmaceutical LTD, MBSTU Caution: Store in a cool and dry place. Keep away from children
|
Precautions
Apron should be worn.
All the instruments were cleaned well. Instruments a were carefully handled.
Volume and weight should be taken carefully.
Ingredients were mixed properly.
Heat should be given carefully.
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