Experiment No: 01 Date: 31.10.2023
Name of the Experiment: Determination of Uniformity of Weight of Paracetamol 500 mg Tablet.
Principle:
The uniformity of the tablet dosage units can be demonstrated by either weight variation or content uniformity test. Weight variation is a compendial test for tablet dosage form and performed when-
If the drug forms greater part of the tablet any variation in the tablet weight obviously indicates a variation in the active ingredient.
Tablet dosage-form uniformly by weight variation is determined by selecting not less than 30 tablets from each production batch and weighing accurately at least 10 tablets individually and calculating the average weight as-
Average weight = Total weight variationNumber of tablet
\ Average weight of tablets X = X1 + X2+ X3….. Xnn
\ % Deviation = Xi-XX ×100 … (1)
Where, i = 1,2,3,……. N
Pharmacopoeial requirements:
Not more than two of the individual tablet weights deviate from the average weight, X by more than the specified limit mentioned in the following table and none deviates by more than twice that %.
Pharmacopoeia | Average weight of tablet | Maximum % deviation |
USP | Tablet less than 120 mg | ± 10 % |
Range from 120-300 mg | ±7.5 % |
More than 300 mg | ± 5.0 % |
BP | 80 mg or less | ± 10 % |
> 80 mg and < 250 mg | ± 7.5 % |
250 mg or more | ± 5.0 % |
Since, the average weight, X of Paracetamol 500 mg is more than 250 mg (according to BP) allowed parent deviation should be ± 5% and not more than two of the individual tablet weights should deviated by. ± 5 % and none should have deviated by 10 %.
Instrumentation:
Procedure:
20 tablets were weighed individually. Then the average weight was calculated and percentage of weight variation was calculated by using equation (1).
% Deviation = X1-XX ×100 … (1)
Where,
Xi = Sample 1, 2, 3,….. 20.
X= Average weight of 20 tablets.
Tablet No. (n) | Individual Weight (Xi) gm | Average weight
X = X1 + X2+ X3….. X2020
| % Deviation
X1-XX ×100 |
1 | 0.6969 | 13.786520
= 0.6893 | 1.102 |
2 | 0.6962 | 1.001 |
3 | 0.6726 | -2.422 |
4 | 0.6883 | -0.1450 |
5 | 0.6874 | -0.276 |
6 | 0.6627 | -3.858 |
7 | 0.6987 | 1.364 |
8 | 0.6978 | 1.233 |
9 | 0.6886 | -0.102 |
10 | 0.6977 | 1.219 |
11 | 0.6899 | 0.087 |
12 | 0.6778 | -1.668 |
13 | 0.6875 | -0.261 |
14 | 0.6964 | 1.030 |
15 | 0.6961 | 0.987 |
16 | 0.6756 | -1.988 |
17 | 0.6960 | 0.972 |
18 | 0.6963 | 1.015 |
19 | 0.6986 | 1.349 |
20 | 0.6854 | -0.566 |
Total weight | 13.7865 |
|
Test Result:
The percent of weight variation ranges from -3.858 to 1.364 %.
No tablet deviated by> ± 5% and this deviation is more or less than ± 10%.
Comments:
The uniformity of weight of 20 tablets complies with the measured specification so the batch can be declared as “passed”.
Precautions:
Weight of all the tablets should be measured carefully.
Apron should be worn in the laboratory.
All the instruments should be handled carefully.
Experiment No: 02 Date: 31.10.2023
Name of the Experiment: Friability test of paracetamol 500mg tablet.
Principle:
Friability is the tendency of the tablet to crumble. It is important for the tablet to resist attrition. Friction and shocks are the forces that most often cause the tablet to chip, cap or break.
The friability test is designed to evaluate the ability of the tablet to withstand abrasion during packaging, handling and shipping. Another application of friability test is to detect incipient capping or laminate when stressed by attrition inside the rotating cylinder present in the friability tester. It is usually measured by the use of Roche friabilator.
A number of tablets is weighed and placed in the apparatus where they are exposed to rolling and repeated shocks as they fall 6 inches in each turn within the apparatus.
The loss due to abrasion is a measure of the tablet friability. The value is expressed as a percentage.
The accepted limit of weight loss after this experiment should not be more than 1 % of the total of the tablets. The percentage of the weight loss can be calculated
by using the following formula.
Instrumentation :
(1) Electronic balance
(2) Roche friabilator
Procedure :
Calculation :
Initial weight of tablets = 6.7709 mg
Final weight of tablets = 6.7608 mg
Percentage of weight loss/friability(%) = 6.7709 - 6.76086.7709 ×100
= 0.14916 %
Result :
The friability of tablets were found 0.14916 % w/w
Comment :
The friability of tablets supplied passed the batch.
Experiment No: 03 Date: 31.10.2023
Name of the Experiment: Determination of hardness of paracetamol 500mg tablet.
Principle:
Tablets should be sufficiently hard to resist breaking during normal handling, packaging, and shipping and yet soft enough to disintegrate properly after swallowing. So the resistance of the tablets to capping, abrasion, or breakage under conditions of storage, transportation, and handling before usage depends on their hardness.
The hardness of the tablets is the non-compendial test and is controlled by the degree of pressure applied during the compression/stage. Hardness is an important criterion since it can affect disintegration and dissolution. If the tablet is too hard, it may not be in the required period of time to meet the dissolution specification. If it is too soft, it may not be able to withstand handling during subsequent processing such as coating or packaging and shipping operations. The test measures crushing strength properly defined as the compressional force applied diametrically to a tablet that just breaks it. The force required to break the tablet is measured in kilograms. A force is about 4 kg is considered the minimum requirement for a satisfactory tablet.
Measuring units:
Most tablet testing is performed using international systems of units. The newton is the preferred unit of force as is recognized by the SI system. However, the kilograms are also used.
(kg) - it is the primary unit of mass recognized by the SI system.
Newton (N) - The newton is the SI unit of force and the unit that should be used for tablet hardness testing 1 kilogram = 9.807 newtonS.
Pound (lb) - technically a unit of mass but can also be used for force.
1 kilogram 2.204 pounds.
Kilo pounds (kp) - it is the unit of force also called a kilogram of force.
Interrelationship of the units:
1kg = 9.807 newtons
1kg = 2.204 pounds
Ikg = 1.4 strong cobs
1kg = 1 kilopound
Instrument used:
Several devices have been used to test the tablet’s hardness.
Monsanto hardness tester
Pfizer Hardness Tester
Strong Cobb Hardness Tester
Procedure:
The tablet to be tested was held between a fixed and moving tank and the reading of the indicator was adjusted to zero. The force applied to the edge of the tablet was gradually increased by moving the screw knob forward until the tablet broke. The reading was noted from the sele/which indicates the required pressure in kg to break the tablet.
Data:
No of Tablet | Hardness in Kg |
1 | 15.67 |
2 | 15.86 |
3 | 16.09 |
4 | 16.56 |
5 | 16.98 |
6 | 17.08 |
Official Standards for Hardness: The hardness of different brands of paracetamol tablets is in the range of 13.67 kg to 26.075 kg
Result: The range of six readings: 15.67 kg to 17.08Kg
Precautions:
Tablet hardness may be affected by -
The speed of testing
The geometry of the tablet contact points
Debris of the testing area
Variation in the temperature humidity
Tablet age, etc .
So, care should be taken.
Experiment No: 04 Date: 31.10.2023
Name of the Experiment: Determination of Disintegration Time of Paracetamol 500mg Tablet.
Principle :
The disintegration test is a measure of the time required under a given set of conditions for a group of tablets to break down into particles which will pass through a mesh screen.
If one or two tablets fail to disintegrate, the test should be repeated using 12 tablets.
Instrumentation :
1. Disintegration tester
2. Glass beaker 1 litre
3. Thermometer
The disintegration tester consists of a basket rack holding 6 plastic tubes, open at the top and bottom. The bottom of the tube is covered by a 10-mesh screen. The basket is immersed in a bat of suitable liquid held at 37°C, preferably in a litre beaker.
Test condition:
Temperature of simulated Gastric fluid: 37°C +0.5
Procedure:
One tablet was placed in each plastic tube and a plastic disc is placed over the tablet. The basket was positioned in one liter beaker containing 900ml gastric fluid at 37°C in such a way that at the highest position of the tube, the screen remains below the surface.
The machine was agitated until the tablet disintegrated. The end point of the test was achieved when no tablet fragment was remaining on the screen. The time of disintegration was recorded.
Data:
No. of tablet | Disintegration time (min-sec) |
|
|
1st tablet | 64 sec |
|
|
2nd tablet | 66 sec |
|
|
3rd tablet | 69 sec |
|
|
4th tablet | 72 sec |
|
|
5th tablet | 68 sec |
|
|
6th tablet | 75 sec |
|
|
Test Result:
The disintegration time of the supplied tablets ranges from 64 to 75 seconds.
Precautions:
Aprons should be worn in the laboratory.
2. All the instruments should be handled carefully.
Experiment No: 05 Date: 31.10.2023
Name of the Experiment: Determination of Dissolution rate of Paracetamol 500 mg Tablets.
Theory:
When a drug administered orally in the form of a tablet, the rate of absorption often controlled how fast the drug dissolved in the GIT fluid of absorption or site.
Drug in solid dosage form in GIT fluid kd→ Drug in solution kd→ Drug in blood → elimination GIT fluid.
Here, Kd represents the rate constant governing dissolution of drug in GI fluid very often Ka Kd and dissolution is the rate-limiting step in the overall absorption process. As a result, the onset of intensity & the duration of action as well as the extent of drug absorption on bioavailability may be altered by changes in the dissolution rate.
The objective of the in vitro dissolution test is as follows:
Whether the drug release is 100% or not.
Whether the rate of drug dissolution is uniform from batch to batch or not.
According to BP & USP the range of percentage release of the drug should be ±5%
Apparatus:
USP dissolution test apparatus
Test tube
Volumetric flask
Filter paper
Pipette
Measuring flask
Spectrophotometer
USP dissolution test apparatus:
It consists of 1000 ml vessel made up of inert transparent material a variable speed motor and a cylindrical dissolution basket. The vessel can be immersed in a suitable cylinder bath at any concentration at size that permits keeping the water continuously in motion and holding the temperature at 37°C ±0.50°C. The basket is detectable and made up of 46 mesh size stainless steel. Set formed into cylinder 3.66 cm height of 25 cm in diameter.
Reagent:
Gastric simulated fluid
N/10 NaoH solution
Distilled water
Preparation of simulated gastric fluid:
2 gm of NaCl and 7 ml of conc. HCl taken in a larger beaker containing distilled water, then the content was transferred in a volumetric flask and the final volume was made to 1000 ml by adding a sufficient amount of distilled water.
Preparation of blank solution:
2 ml of gastric simulated fluid was taken into a 10 ml volumetric flask and 0.1 N NaOH was added to it. It was the blank solution.
Preparation of standard solution:
Each paracetamol, tablet Contain 500mg active ingredient
Paracetamol BP. A tablet was dissolved in 1000ml fluid so,
1000ml fluid contains 500 mg of paracetamol
1ml fluid contain 5001000 mg of paracetamol
100 ml fluid contain 50 mg of paracetamol
Procedure:
The beaker was filled with 1000ml gastric simulated fluid & the fluid was heated up to 37°C by adjusting the temperature.
The tablet was put into the beaker & the instrument was stirred immediately, the speed of the stirrer was 50 ppm.
After 30 minutes 100ml of sample from the beaker was taken in a test tube & filtered.
2ml of filtered taken and 0.1N NaOH added to it up to 100 ml and it was sample solution.
Approximately 50 mg (0.05gm) paracetamol was dissolved in gastric fluid and was made 100 ml with it. 10 ml was taken from the solution & was filtered.
From the filtrate 2 ml was taken in a measuring flask & 0.1N NaOH was added to make the volume 100 ml. It was the standard solution.
Now the absorbance of blank solution sample solution & standard solution was taken 254 m in the spectrometer. At first, the absorbance of the blank solution was taken and the apparatus was done auto zero/So this reading is not necessary after the reading the absorbance of sample standard was taken then, the percentage of content of paracetamol in the solution was calculated.
Calculations:
1000 ml simulated fluid contains 500 mg of paracetamol
1ml simulated fluid contains 0.5 mg of paracetamol
Therefore, the concentration of standard solution was .5 mg/ml of paracetamol. Concentration of sample solution can be calculated by using the following formula:
As/Astd = Cs/Cstd
Cs=AsCstdAstd
=0.585×0.50.62
=0.4714
Where, C is concentration of sample solution =0.4714
Concentration of standard solution = 0.5 mg/ml
Absorbance of the sample solution As=3.5086 = 0.585
Absorbance of standard solution Astd=0.62
Now,
Then multiplication with 1000,
=0.4717×1000
= 471.7
We know that % release of drug =471.7500×100
=94.34%
Results:
Percentage release of paracetamol was 94.34%
Precautions:
Apron must be worn.
All the instruments must be handled carefully
All the measurement should be done accurately
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