## STP FOR CALCIUM AND VITAMIN D3 TABLETS

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:

1. In the assay, the retention time of principal peak in the chromatogram obtained with the test solution corresponds to the peak in the chromatogram obtained with the reference solution.
2. Disperse a quantity of powdered tablets containing 10 mg of calcium in 50ml of water and filter. It gives the reaction (A) of calcium salts.

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:

Medium: 900ml of 0.1 M HCl

Time: 30 minutes

Speed: 75 rpm

Limit: NLT 75% of the stated amount of Aceclofenac.

Withdraw a suitable volume of the medium and filter the solution through a filter paper (whatman No.1), collect the solution through a filtrate. Transfer 20ml of this solution in to 250ml volumetric flask, add 150ml of water, and add 3ml of 1 M sodium hydroxide and 10ml of ammonia solution. Titrate with 0.05M disodium edentate, using hydroxyl napthol blue as an indicator. Carry out a blank titration.

1 ml of 0.5 M disodium edentate is equivalent to 0.002004g of calcium.

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 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.

10.0)    Uniformity of content: Determined by liquid chromatography.

Test solution: Disperse one tablet in 8ml of methanol with the aid of ultrasound for 15 minutes, dilute to 10.0ml with methnol, mix and centrifuge. Use the supernatant liquid.

Reference solution: A 0.00005 per cent w/v solution of cholecalciferol reference standard in the methanol.

Chromatographic system:

• A stainless steel column 10cmX4.6mm packed with octadecylsilane bonded to porous silica polymer (5µm)
• Mobile phase: a mixture of 3 volumes of water and 97 volumes of methanol
• Flow rate: 1ml per minute,
• Spectrophotometer set at 264nm,
• Injection volume: 50µl

Calculate the content of vitamin D3 in the tablet.

11.0)    Assay: Determined by liquid chromatography.

For Calcium:

Weigh and powder 20 tablets. Weigh quantity of the powder containing equivalent to 50mg of calcium add 50.0ml of water and 5ml of HCl. Heat the dispersion gently to boiling and continue to boil for about 2 minutes. Allow to cool and add 50ml of 0.05 M disodium edentate. Neutralise the solution using 2 M sodium hydroxide, add 10ml of ammonia buffer pH 10.9 and 50ml of water. Titrate the excess of disodium edentate with 0.05 M zinc chloride using mordant black II solution as indicator.

Carry out a blank titration.

1ml of 0.05 M disodium edentate is equivalent to 0.002004 g of Calcium.

Calculate the content of Calcium in the tablets.

For Vitamin D3 (Cholecalciferol)

Note: Use low-actinic glassware throughout the procedure.

Test solution: Weigh and powder 20 tablets. Disperse a quantity of powdered tablet equivalent to 0.1mg of vitamin D3 in 170ml of methanol by shaking for 5 minutes and mix with ultrasound for 5 minutes, dilute to 200.0ml with methanol, mix and filter. Use the filtrate.

Reference solution: A 0.00005 per cent w/v solution of cholecalciferol reference standard in the methanol.

Chromatographic system:

• A stainless steel column 10cmX4.6mm packed with octadecylsilane bonded to porous silica polymer (5µm)
• Mobile phase: a mixture of 3 volumes of water and 97 volumes of methanol
• Flow rate: 1ml per minute,
• Spectrophotometer set at 264nm,
• Injection volume: 50µl

Inject the reference solution and the test solution.

Calculate the content of Vitamin D3 in the tablet.

Acceptance criteria: 90.0%-110.0%

12.0)    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