1.0) Description: Visual
2.0) 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.
Tablets were weighed individually and the percentage of deviation of its weight from the average weight was determined for each tablet. Formula for calculate the percentage of deviation = (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% |
4.0) Identification Test:
- Extract a quantity of the powdered tablets containing 0.2g of flavoxate HCl with 10ml of dichloromethane, filter and evaporate the filtrate to dryness. On the residue, determine by infrared absorption spectrophotometry. Compare the spectrum with that obtained with flavoxate HCl reference standard with the reference spectrum of flavoxate HCl.
- In the test for related substances, by applying 10µl of each solution, the principal spot in the chromatogram obtained with test solution (b) corresponds to that in the chromatogram obtained with reference solution (c).
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) 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 upto 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.
9.0) Related substances:
Determine by thin layer chromatography, coating the plate with silica gel GF254.
Mobile phase: A mixture of 1 volume of 18 M ammonia, 80 volumes of propan-2-ol and 200 volumes of ethyl acetate.
Test solution (a): Disperse a quantity of the powdered tablets containing 0.2 g of flavoxate HCl with 10ml of chloroform and filter.
Test solution (b): Dilute 1ml of test solution (a) to 20ml with chloroform.
Reference solution (a): A 0.015 per cent w/v solution of 3-methylflavone-8-carboxylic acid ethyl ester reference standard in chloroform.
Reference solution (b): Dilute 1ml of test solution (a) to 500ml with chloroform.
Reference solution (c): A 0.1 per cent w/v solution of flavoxate HCl reference standard in chloroform.
Reference solution (d): A 0.03 per cent w/v solution of 3-methylflavone-8-carboxylic acid reference standard in chloroform.
Apply 10µl of reference solution (a), (c), (d), test solution (b), 25µl of reference solution (b) and 50µl of test solution (a). After removal of the plate, allow it to dry in air and examine under ultraviolet light at 254nm. Any spot corresponding to 3-methylflavone-8-carboxylic acid ethyl ester in the chromatogram obtained with test solution (a) is not more intense than the spot in the chromatogram obtained with reference solution (a) (0.15 per cent) and any other secondary spot in the chromatogram obtained with test solution (a), other than the spot corresponding to 3-methylflavone-8-carboxylic acid is not more intense than the spot in the chromatogram obtained with reference solution (b) (0.1 per cent).
10.0) 3-Methylflavone-8-carboxylic acid:
Determine by thin layer chromatography, coating the plate with silica gel GF254.
Mobile phase: A mixture of 4 volumes of glacial acetic acid, 25 volumes of ethyl acetate and 70 volumes of cyclohexane.
Test solution: Disperse a quantity of the powdered tablets containing 0.2 g of flavoxate HCl with 10ml of chloroform and filter.
Reference solution: A 0.01 per cent w/v solution of 3-methylflavone-8-carboxylic acid reference standard in chloroform.
Apply 50µl of each solution. After removal of the plate, allow it to dry in air and spray with dilute potassium iodobismuthate solution. Any spot corresponding to 3-methylflavone-8-carboxylic acid in the chromatogram obtained with the test solution is not more intense than the spot in the chromatogram obtained with the reference solution (0.5 per cent).
11.0) Assay: Determined by liquid chromatography.
Weigh and powder 20 tablets. Disperse a quantity of powder containing 1g of flavoxate HCl with 600ml of 0.1 M HCl with the aid of ultrasound for 10 minutes. Place in a water bath at 70° for 90 minutes, cool and dilute 1000ml with 0.1 M HCl. Dilute 5ml of 250ml with 0.1 M HCl and measure the absorbance at 293nm. Calculate the content of Flavoxate HCl from the absorbance obtained by using a 0.002 per cent w/v solution of Flavoxate HCl reference standard in 0.1 M HCl.
Acceptance criteria: 95.0%-105.0%
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:
Wt.: Weight
mg: Miligram
ml: Milileter
STD: Standard
inHg: Inch of Mercury
rpm: Rounds per minute
CFU: Colony forming unit
HCl: hydrochloric acid
