1.0) Description: Visual
2.0) Average Weight: Check weight of 20 tablets at randomly and calculate the average weight by formula.
Average weight (mg) = wt of 20 tablets (gm) x 1000
20
3.0) Uniformity of weight:
Weigh 20 tablets selected at random and calculate the average weight. Not more than two of the individual weights deviate from the average weight by more than the percentage shown in table.
Tablets were weighed individually and the percentage of deviation of its weight from the average weight was determined for each tablet. Formula to calculate the percentage of deviation.
Deviation (%) = Weight of each tablet – Average weight x 100
Average weight
| Average weight of tablets | Percentage deviation |
| More than 80mg but Less than 250mg | ±7.5% |
4.0) Identification Test:
In the assay, the principal peak in the chromatogram obtained with the test solution corresponds to the peak in the chromatogram obtained with the reference solution.
5.0) Hardness:
The standard method used for tablet hardness testing is compression testing. The tablet is placed between two jaws that crush the tablet. The machine measures the force applied to the tablet and detects when it fractures.
6.0) Disintegration Time:
Unless otherwise stated in the individual monograph, introduce one tablet into each tube and add a disc to each tube. The assembly is suspended in the liquid medium in a suitable vessel, preferably a 1-litre beaker. The volume of liquid is such that the wire mesh at its highest point is at least 15mm below the surface of the liquid, and at its lower point is at least 25mm above the bottom of the beaker. At no time should the top of the basket-rack assembly become submerged. There is a thermostatic arrangement for heating the liquid and maintaining the temperature at 37±2°.
If 1 or 2 tablets fail to disintegrate, repeat the test on 12 additional tablets; not less than 16 of the total of 18 tablets tested disintegrate.
If the tablets adhere to the disc and the preparation under examination fails to comply, repeat the test omitting the disc. The preparation complies with the test if all the tablets in the repeat test disintegrate.
7.0) Dimension of Tablet:
Length, breadth, and thickness or diameter in round tablet are determined by vernier calliper in mm.
8.0) Friability:
The test is applicable to compressed tablets and is intended to determine the physical strength of tablets. Tablets with a unit weight equal to or less than 650 mg, take a sample of whole tablets corresponding as near as possible to 6.5 g. For tablets with a unit weight of more than 650mg, take a sample of 10 whole tablets. The tablets should be carefully dedusted prior to testing. Accurately weigh the tablet sample, and place the tablets in the drum. Rotate the drum 100 times and remove the tablets. Remove any loose dust from the tablets as before, and accurately weigh.
The test is run only once unless the results are difficult to interpret or if the weight loss is greater than the target value, in which case, the test is repeated twice and the mean of the three tests is determined.
% Friability = W1 – W2 X 100
W1
W1= Initial weight W2= Final weight
A maximum loss of weight (From a single test or from the mean of three tests) not greater than 1.0 percent is acceptable for most tablets.
If obviously cracked, chipped or broken tablets are present in the sample after tumbling, the sample fails the test.
9.0) Dissolution:
Apparatus: Paddle
Medium: 900 ml of 0.1 M HCl (51 ml concentrated HCl in 6000 ml water)
Speed: 100 rpm
Time: 45 minutes
Withdraw a suitable volume of the medium and filter. Measure the absorbance of the filtrate, suitably diluted with the dissolution medium if necessary, at the maximum at about 230 nm. Calculate the content of Cetirizine HCl in the medium from the absorbance obtained from a solution of known concentration of Cetirizine HCl reference standard in the same medium.
Formula:
Abs. of test
—————– X STD Dilution X Test Dilution X Potency of STD X 100
Abs. of STD
Limit: N.L.T. 80% of the stated amount of Cetirizine HCl.
10.0) Leak test:
The apparatus is used to test for the integrity of packed strips, blisters and Alu-Alu Blister pack containing tablets. Ensure apparatus bath is filled with purified water up to mark indicated and add 0.5% crystal violet solution in water. Samples are placed into the desiccators and the lid is placed in position. The pump starts to produce a vacuum 15inHg inside the desiccators and the vacuum is held for 1 minute. The sample remains at the required vacuum level for given time interval buzzer will sound after time is over and will cut off the vacuum pump. As the package is immersed in a colored dye solution the venting of the desiccators will allow any holes to be penetrated by the dye and the contents of the flexible packaging will also be stained with the same coloring material.
Examine all the strips for any leakage by opening the pockets manually. If anyone pocket shows evidence of leakage, reject the sample, stop the Blister / Strip machine and immediately take corrective action.
11.0) Related substances: Determine by liquid chromatography.
Test solution: Weigh and powder 20 tablets. Weigh accurately a quantity of the powder containing 20 mg of Cetirizine HCl, add 50 ml of the mobile phase, mix and dilute to 100 ml with the mobile phase.
Reference solution (a): A solution containing 0.02 per cent w/v each of Cetirizine HCl reference standard and (RS)-1-[(4-chlorophenyl) phenylmethyl] piperazine reference standard (Cetirizine impurity A) in the mobile phase. Dilute 1 ml of the solution to 100 ml with the mobile phase.
Reference solution (b): Dilute 1.0 ml of the test solution to 100.0 ml with the mobile phase.
Chromatographic system:
- A stainless steel column 25 cm X 4.6 mm, packed with silica gel (5µl),
- Mobile phase: a mixture of 0.4 volume of dilute sulphuric acid, 6.6 volumes of water and 93 volumes of acetonitrile,
- Flow rate: 1 ml per minute.
- Spectrophotometer set at 230 nm,
- Injection volume: about 20 µl
Inject reference solution (a). The test is not valid unless the resolution between the peaks due to Cetirizine and Cetirizine impurity A is not less than 2.0 and tailing factors not more than 2.0.
Inject reference solution (b) and the test solution. Run the chromatogram 3 times the retention time of Cetirizine. In the chromatogram obtained with the test solution the area of any impurity peak is not more than 0.5 times the area of the principal peak in the chromatogram obtained with reference solution (b) (0.5 per cent). The sum of areas of all such peaks is not more than the area of the principal peak in the chromatogram obtained with reference solution (b) (1.0 per cent). Ignore any peak with an area 0.05 times the area of the principal peak in the chromatogram obtained with reference solution (b) (0.05 per cent).
12.0) Uniformity of content: (For tablets containing 10 mg or less)
Test solution: Disperse 1 tablet in the mobile phase, mix and dilute to 100 ml with the mobile phase, filter. Dilute 5 ml of the solution to 100 ml with mobile phase.
Reference solution: A 0.05 per cent w/v solution of Cetirizine HCl reference standard in the mobile phase. Dilute 1.0 ml of the solution to 10.0 ml with the mobile phase.
Chromatographic system:
- A stainless steel column 25 cm X 4.6 mm, packed with octadecylsilane chemically bonded to porous silica (5 µm),
- Mobile phase: Dissolve 0.19 g of heptanes sulphonic acid sodium salt in 300 ml water add 700 ml acetonitrile and mix. Adjust pH to 3.2 with 0.05 M sulphuric acid, filter.
- Flow rate: 1.2 ml per minute,
- Spectrophotometer set at 230 nm,
- Injection volume: 20 µl
13.0) Assay: Determined by liquid chromatography.
Test solution: Weigh and powder 20 tablets. Weigh accurately a quantity of the powder containing about 25 mg Cetirizine HCl, add the mobile phase, mix and dilute to 50.0 ml with the mobile phase, filter. Dilute 1.0 ml of the solution to 10.0 ml with the mobile phase.
Reference solution: A 0.05 per cent w/v solution of Cetirizine HCl reference standard in the mobile phase. Dilute 1.0 ml of the solution to 10.0 ml with the mobile phase.
Chromatographic system:
- A stainless steel column 25 cm X 4.6 mm, packed with octadecylsilane chemically bonded to porous silica (5µm),
- Mobile phase: Dissolve 0.19 g of heptanes sulphonic acid sodium salt in 300 ml water add 700 ml acetonitrile and mix. Adjust pH to 3.2 with 0.05 M sulphuric acid, filter.
- Flow rate: 1.2 ml per minute,
- Spectrophotometer set at 230 nm,
- Injection volume: 20 µl
Inject the reference solution. The test is not valid unless the tailing factor is not more than 2.0, the column efficiency is not less than 2000 theoretical plates and the relative standard deviation for replicate injections is not more than 2.0 per cent.
Inject the reference solution and the test solution.
Calculate the content of Cetirizine HCl in the tablets.
Formula:
Area of Test STD Wt.(mg) 1 50 10 Potency
—————–X—————–X——-X—————X——–X———–X Average wt.
Area of STD 50 10 Test Wt.(mg) 1 100
Alternative Method: By UV Spectrophotometer
Test Solution: Weigh and powder 20 tablets. Weight sample equivalent to 25 mg of Cetirizine HCl 100 ml volumetric flask add 20 ml 0.1 M HCl into it and sonicate to dissolve the test sample. Make up to mark with 0.1 M HCl. Filter and dilute 2 ml of this solution to 50 ml in same 0.1 M HCl.
Reference Solution: Weigh 25 mg of reference standard of Certirizine HCl in 100 ml of volumetric flask. Add 20 ml 0.1 M HCl into it and sonicate to dissolve. Dilute 2 ml of this solution to 50 ml with 0.1 M HCl.
Check Absorbance of test as well as reference standard at about 232 nm in UV Spectrophotometer.
Calculate the content of Cetirizine HCl in the tablets.
Formula:
Abs. of Test STD Wt.(mg) 2 100 50 Potency
—————–X——————X——-X—————X——–X———–X Average wt.
Abs. of STD 100 50 Test Wt.(mg) 2 100
Acceptance criteria: 90.0%-110.0%
14 .0) MICROBIOLOGICAL PURITY
Perform the test according to requirements of IP,
Total aerobic Microbial count (TAMC): NMT 103 CFU/g
Total combined yeasts/Moulds count (TYMC): NMT 102 CFU/g
Pathogens: in 1gm drug.
Escherichia Coli – Should be absent
Pseudomonas aeroginosa – Should be absent
Salmonella – Should be absent
Staphylococcus aureus– Should be absent
Abbreviations:
Wt.: Weight Abs. Absorbance
ml: Millilitre STD: Standard
inHg: Inch of Mercury rpm: Rotations per minute
CFU: Colony forming unit Abs.: Absorbance
w/v:Weight/Volume
mg: Milligram
HCl: Hydrochloric acid
