STP FOR ESCITALOPRAM 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:

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:

Medium: 900ml of 0.1 M hydrochloric acid.

Speed: 50rpm

Time: 45 minutes

Limit: NLT 75% of the labeled amount of Escitalopram is dissolved.

Withdraw a suitable volume of the medium and filter.

Determine by liquid chromatography.

Test solution: The filtrate obtained as given above, diluted if necessary with the dissolution medium.

Reference solution: A solution of escitalopram oxalate referenec standard containing about 0.00055 per cent w/v of escitalopram in the dissolution medium.

Chromatographic system:

• A stainless steel column 25cm X4.6mm, packed with octylsilane bonded to porous silica (5µm),
• Mobile Phase: a mixture of 45 volumes of buffer solution prepared by dissolving 3.7 g of disodium hydrogen phosphate dihdrate in 1000ml of water, adjusted to pH 7.0 with O.P.A., 27.5 volumes of methanol and 27.5 volumes of acetonitrile,
• Flow rate: 1.5ml per minute,
• Spectrophotometer set at 226nm,
• Injection volume: 20µl

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, as described under assa using following solution as the test solution.

Test solution: Disperse 1 tablet in the mobile phase, sonicate and dilute, if necessary to obtain a solution containing 0.001 per cent w/v of escitalopram in the mobile phase.

11.0)    Assay: Determined by liquid chromatography.

Test solution: Weigh and powder 20 tablets. Disperse a quantity of powder containing 25mg of escitalopram with 30ml of mobile phase, sonicate to dissolve and dilute to 50.0ml with the mobile phase. Further dilute to obtain a 0.001per cent w/v solution of escitalopram.

Reference solution: A solution of escitalopram oxalate reference standard containing about 0.001 per cent w/v of escitalopram in the mobile phase.

Chromatographic system:

• A stainless steel column 25cm X4.6mm, packed with octylsilane bonded to porous silica (5µm),
• Mobile Phase: a mixture of 45 volumes of buffer solution prepared by dissolving 3.7 g of disodium hydrogen phosphate dihdrate in 1000ml of water, adjusted to pH 7.0 with O.P.A., 27.5 volumes of methanol and 27.5 volumes of acetonitrile,
• Flow rate: 1.5ml per minute,
• Spectrophotometer set at 226nm,
• Injection volume: 20µl

Inject the reference solution. The test is not valid unless the theoretical plates is not less than 40000, the tailing factor is not more than 2.0 and the relative standard deviation for replicate injections is not more than 2.0 per cent.

Inject reference solution and the test solution.

Calculate the content of Escitalopram in the tablets.

Alternative Method: By UV Spectrophotometer

Test Solution: Weigh and powder 20 tablets. Weight sample equivalent to 10mg of Escitalopam oxalate in 100ml volumetric flask add l0ml 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 5ml of this solution to 50ml in same solvent.

Reference Solution: Weigh 50mg of reference standard of escitalopram in 100ml of volumetric flask. Add 10ml 0.1 M HCl into it and sonicate to dissolve. Make up to mark with 0.1 M HCl. Dilute 1ml of this solution to 50ml with same solvent.

Check Absorbance of test as well as reference standard at 239nm in UV Spectrophotometer.

Calculate the content of Escitalopram.

Formula for calculation:

Absorbance of TEST       STD wt. (mg)      1            100              50        Potency

—————————-X——————–X———X————–X———X———–X Avg. Wt.

Absorbance of STD            100                 50       Test wt (mg)      5           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:

Wt.: Weight

mg: Miligram

ml: Milileter

STD: Standard

inHg: Inch of Mercury

rpm: Rounds per minute

CFU: Colony forming unit

O.P.A.: Orthophosphoric acid

w/v: Weight/volume

HCl: Hdrochloric acid