- Description: Visual
- Average Weight: Check weight of 20 tablets at randomly and calculate the average weight by formula : wt of 20 tablets (gm) x 1000 / 20. found avg. wt in mg
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.
Weigh the tablets individually and calculate the percentage of deviation for each tablet. By using formula = (experimental weight – theoretical weight) x 100%
Theoretical weight
| Average weight of tablets | Percentage deviation |
| More than 80mg but Less than 250mg | 7.5% |
| 250mg or More | 5% |
- 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. Although compressive force is applied to the tablet, along the diameter of the tablet at right angles to the applied force.
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 are determined by vernier in mm
8.0) Dissolution:
Apparatus: Paddle
Medium: 900ml of phosphate buffer 6.8 pH
Speed: 50 rpm
Time: 30 minutes
Limit: NLT 80% of the labeled amount of Levocetirizine DiHCl is dissolved.
Withdraw a suitable volume of the medium and filter.
Determine by liquid chromatography.
Test solution: Use the filtrate.
Reference solution: A 0.025 per cent w/v solution of levocetirizine DiHCl reference standard in mobile phase. Dilute 1ml of the solution to 50ml with dissolution medium.
Chromatographic system:
- A stainless steel column 25cm X4.6mm, packed with octadecylsilane chemically bonded to porous silica (5µm).
- Mobile phase: a mixture of 60 volumes of 0.05 M potassium dihydrogen phosphate and 40 volumes of acetonitrile, adjust the pH to 6.0 with 10 per cent w/v of sodium hydroxide.
- Flow rate: 1ml per minute.
- Spectrophotometer set at 230nm,
- Injection volume: about 20µl
Calculate the content of Levocetirizine DiHCl in tablets.
9.0) 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.
10.0) Related substances:
Determined by liquid chromatography.
Test solution: Weigh and powder 20 tablets. Weigh a quantity of the powdered tablet containing 25mg of levocetirizine diHCl, dissolve in 25ml of mobile phase.
Reference solution (a): A 0.1 per cent w/v solution of levocetirizine HCl reference standard in mobile phase.
Reference solution (b): Dilute 1ml of reference solution (a) to 100ml with mobile phase.
Chromatographic system:
- A stainless steel column 25cm X4.6mm, packed with octadecylsilane chemically bonded to porous silica (5µm).
- Mobile phase: a mixture of 60 volumes of 0.05 M potassium dihydrogen phosphate and 40 volumes of acetonitrile, adjust the pH to 6.0 with 10 per cent w/v of sodium hydroxide.
- Flow rate: 1ml per minute.
- Spectrophotometer set at 230nm,
- Injection volume: about 20µl
Inject reference solution (a). Test is not valid unless the column efficiency is not less than 2000 theoretical plates and tailing factor is not more than 2.0.
Inject reference solution (b) and test solution. In the chromatogram obtained with the test solution, the area of any secondary peak is not more than the peak in the chromatogram obtained with reference solution (b) (1.0 per cent) and the sum of area of all the secondary peaks is not more than twice the area of the peak in the chromatogram obtained with the reference solution (b) (0.2 per cent).
11.0) Uniformity of content:
Test solution: transfer 1 tablet in a suitable volumetric flask, add about 20ml of mobile phase to disperse with shaking. Further dilute with the mobile phase to obtain a final concentration of 0.0025 per cent w/v.
Reference solution: A 0.0025 per cent w/v solution of levocetirizine diHCl reference standard in the mobile phase.
Chromatographic system:
- A stainless steel column 25cm X4.6mm, packed with octadecylsilane chemically bonded to porous silica (5µm).
- Mobile phase: a mixture of 60 volumes of 0.05 M potassium dihydrogen phosphate and 40 volumes of acetonitrile, adjust the pH to 6.0 with 10 per cent w/v of sodium hydroxide.
- Flow rate: 1ml per minute.
- Spectrophotometer set at 230nm,
- Injection volume: about 20µl
12.0) Assay: Determined by liquid chromatography.
Test solution: Weigh and powder 20 tablets. Weigh accurately a quantity of the powdered tablet containing 25mg of levocetirizine DiHCl, disperse in 100ml of mobile phase and filter. Dilute 5ml of the solution to 25ml with mobile phase.
Reference solution: A 0.005 per cent w/v solution of Levocetirizine DiHCl.
Chromatographic system:
- A stainless steel column 25cm X4.6mm, packed with octadecylsilane chemically bonded to porous silica (5µm).
- Mobile phase: a mixture of 60 volumes of 0.05 M potassium dihydrogen phosphate and 40 volumes of acetonitrile, adjust the pH to 6.0 with 10 per cent w/v of sodium hydroxide.
- Flow rate: 1ml per minute.
- Spectrophotometer set at 230nm,
- Injection volume: about 20µl
Inject reference solution. The test is not valid unless the tailing factor is not more than 2.0. The column efficiency is not less than 1500 theoretical plates. The relative standard deviation for replicate injections is not more than 2.0 per cent.
Inject the reference solution and test solution.
Calculate the content of Levocetirizine Dihydrochloride in the tablets.
Alternative Method: By UV Spectrophotometer
Test Solution: Weigh and powder 20 tablets. Weight sample equivalent to 25mg of Levocetirizine DiHCl 100ml volumetric flask add 20ml 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 2ml of this solution to 50ml in 0.1 M HCl.
Reference Solution: Weigh 25mg of reference standard of Levocetirizine DiHCl in 100ml of volumetric flask. Add 20ml 0.1 M HCl into it and sonicate to dissolve. Make up to mark with 0.1 M HCl. Dilute 2ml of this solution to 50ml with 0.1 M HCl.
Check Absorbance of test as well as reference standard at about 230nm in UV Spectrophotometer.
Calculate the content of Levocetirizine DiHCl 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%
13.0) 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:
mg: Miligram
ml: Milileter
inHg: Inch of Mercury
rpm: Rounds per minute
CFU: Colony forming unit
HCl: Hydrochloric acid
w/v: Weight/volume
