standard testing procedure domperidone

Storage Requirements:
Store protected from light.

Sampling:
Sample equal quantity from each container / bag. Collect a minimum of 5g from each container/bag sample into individual, self –sealing polythene bag kept in another self sealing polythene bag bearing ‘Sample for analysis, label. After completion of sampling return rest sample on same container. Collect control sample in Pet Bottle/Glass Bottle.

Quantity of Composite Sample:

10 g

Quantity of individual Identification
0.0100 g from each and every container /bag.

Quantity of Control Sample:

2 X 10 g

Description: A white or almost white powder.

Solubility: Soluble in dimethylformamide; slightly soluble in ethanol (95per cent) and in methanol; practically insoluble in water.

Identification: By IR.

Appearance of solution: A 1.0% solution in dimethylformamide is clear (2.4.1) and not more intensely coloured than reference solution YS6.

Related Substances: Determine by liquid chromatography.
A. Single impurity: Not more than 0.25%.
B. Total impurity: Not more than 0.50%.

Heavy Metals: NMT 20ppm.

Sulphated Ash: NMT 0.10%w/w.

Loss on drying: NMT 0.5%w/w.

Assay: 99.0% to 101.0%w/w on the dried basis.

Description: A white or almost white powder.
Examine the individual samples by visually.

Reporting: Report as Complies/Does not comply.

Solubility: Soluble in dimethylformamide; slightly soluble in ethanol (95per cent) and in methanol; practically insoluble in water.

Reporting: Report as Complies/Does not comply.

Identification:

Determine by infrared absorption spectrophotometry. Compare the spectrum with that obtained with domperidone RS or with reference spectrum of domperidone.

Reporting: Report as Complies/Does not comply.

Appearance of solution: A 1.0% solution in dimethylformamide is clear (2.4.1) and not more intensely coloured than reference solution YS6

Reporting: Report as Complies/Does not comply.

Related Substances: Determine by liquid chromatography.

Test Solution: Dissolve 0.1 g of the substance under examination in dimethylformamide and dilute to 10.0 ml with the same solvent.

Reference Solution (a): A solution containing 0.01 per cent w/v of domperidone RS and 0.015 per cent w/v of droperidol RS in dimethylformamide.

Reference Solution (b): Dilute 1.0 ml of the test solution to 100 ml with dimethylformamide. Dilute 5.0 ml of the solution 20 ml with dimethylformamide.

Where,
Imp. = Impurity.

Heavy Metals:

Standard solution: Into a 50-ml Nessler cylinder pipette 1.0 ml of lead standard solution (20 ppm Pb) and dilute with water to 25 ml. Adjust with dilute acetic acid or dilute ammonia solution to a pH between 3.0 and 4.0, dilute with water to about 35 ml and mix.

Test solution: Weigh in a suitable crucible the 1.0 gm of the sample, add sufficient sulphuric acid to wet the sample, ignite carefully at a low temperature until thoroughly charred. Add to the charred mass: 2 ml of nitric acid and 5 drops of sulphuric acid and heat cautiously until white fumes are no longer evolved. Ignite, preferably in a muffle furnace, at 500º to 600º, until the carbon is completely burnt off. Cool, add 4 ml of hydrochloric acid, cover” digest on a water-bath for 15 minutes, uncover and slowly evaporate to dryness on a water-bath. Moisten the residue with 1 drop of hydrochloric acid, add 10 ml of hot water and digest for 2 minutes. Add ammonia solution drop wise until the solution is just alkaline to litmus paper, dilute to 25 ml with water and adjust with dilute acetic acid to a pH between 3.0 and 4.0. Filter, If necessary, rinse the crucible and the filter with 10 ml of water, combine the filtrate and washings in a 50-ml Nessler cylinder, dilute with water to about 35 ml and mix.

Procedure: To each of the cylinders containing the standard solution and test solution respectively add 10 ml of freshly
prepared hydrogen sulphide solution, mix, dilute to 50 ml with water, allow to stand for 5 minutes and view downwards over a white surface; the colour produced with the test solution is not more intense than that produced with the standard
solution.

Reporting: Report as ppm.