Domperidone Tablets

General Notices

Action and use

Peripheral dopamine receptor antagonist; antiemetic.

Definition

Domperidone Tablets contain Domperidone Maleate.

The tablets comply with the requirements stated under Tablets and with the following requirements.

Content of domperidone, C22H24ClN5O2

95.0 to 105.0% of the stated amount.

Identification

A. Carry out the method for thin-layer chromatography, Appendix III A, using the following solutions in a mixture of equal volumes of dichloromethane and methanol.
(1) Shake a quantity of the powdered tablets containing the equivalent of 10 mg of domperidone with 10 mL of solvent and filter through a glass microfibre filter (Whatman GF/C is suitable).
(2) 0.127% w/v of domperidone maleate BPCRS.
chromatographic conditions
(a) Use a precoated silica gel F254 plate (Merck silica gel 60 F254 plates are suitable).
(b) Use the mobile phase as described below.
(c) Apply 10 µL of each solution.
(d) Develop the plate to 15 cm.
(e) After removal of the plate, dry in air and examine under ultraviolet light (254 nm). Spray the plate with potassium iodobismuthate solution and examine again.
mobile phase

5 volumes of a solution prepared by dissolving 1.36 g of sodium acetate in 50 mL of water, adjusting the pH to 4.7 with dilute acetic acid and adding sufficient water to produce 100 mL, 18 volumes of methanol, 23 volumes of dichloromethane and 54 volumes of ethyl acetate.

confirmation

Using each method of visualisation, the principal spot in the chromatogram obtained with solution (1) corresponds to that in the chromatogram obtained with solution (2).

B. In the Assay, the principal peak in the chromatogram obtained with solution (1) has the same retention time as the principal peak in the chromatogram obtained with solution (2).

TESTS

Dissolution

Comply with the requirements for Monographs of the British Pharmacopoeia in the dissolution test for tablets and capsules, Appendix XII B1.

test conditions
(a) Use Apparatus 2, rotating the paddle at 50 revolutions per minute.
(b) Use 900 mL of 0.1m hydrochloric acid, at a temperature of 37°, as the medium.
procedure
(1) After 45 minutes withdraw a 20 mL sample of the medium and measure the absorbance of the filtered sample, suitably diluted with the dissolution medium if necessary, at the maximum at 286 nm, Appendix II B using dissolution medium in the reference cell.
(2) Measure the absorbance of a 0.001% w/v solution of domperidone maleate BPCRS in the dissolution medium using dissolution medium in the reference cell.
determination of content

Calculate the total content of domperidone, C22H24ClN5O2, in the medium from the absorbances obtained and using the declared content of C22H24ClN5O2, in domperidone maleate BPCRS.

Related substances

Carry out the method for liquid chromatography, Appendix III D, using the following solutions prepared immediately before use.

(1) To a quantity of the powdered tablets containing the equivalent of 50 mg of domperidone add 10 mL of a mixture of equal volumes of 0.01m hydrochloric acid and methanol, mix with the aid of ultrasound for 20 minutes and filter through a glass microfibre filter (Whatman GF/C is suitable).
(2) Dilute 1 volume of solution (1) to 200 volumes with a mixture of equal volumes of 0.01m hydrochloric acid and methanol. Dilute 1 volume of the resulting solution to 2 volumes with the same solvent.
(3) Dilute 1 volume of solution (2) to 5 volumes of a mixture of equal volumes of 0.01m hydrochloric acid and methanol.
(4) 0.01% w/v of domperidone maleate BPCRS and 0.015% w/v of droperidol EPCRS in a mixture of equal volumes of 0.01m hydrochloric acid and methanol.
chromatographic conditions
(a) Use a stainless steel column (10 cm × 4.6 mm) packed with base-deactivated, end-capped octadecylsilyl silica gel for chromatography (3 µm) (Hypersil BDS is suitable).
(b) Use gradient elution and the mobile phase described below.
(c) Use a flow rate of 1.5 mL per minute. Equilibrate the column for at least 30 minutes with methanol and equilibrate with the initial mobile phase for at least 5 minutes.
(d) Use an ambient column temperature.
(e) Use a detection wavelength of 280 nm.
(f) Inject 10 µL of each solution. Inject a mixture of equal volumes of 0.01m hydrochloric acid and methanol as a blank prior to the solutions.
mobile phase
Mobile phase Amethanol.
Mobile phase B0.5% w/v solution of ammonium acetate.
system suitability

The test is not valid unless, in the chromatogram obtained with solution (4), the resolution between the two principal peaks is at least 2.

limits

In the chromatogram obtained with solution (1):

the area of any secondary peak is not greater than the area of the principal peak in the chromatogram obtained with solution (2) (0.25%);

the sum of the areas of any secondary peaks is not greater than twice the area of the principal peak in the chromatogram obtained with solution (2) (0.5%).

Disregard any peak in the chromatogram obtained with the blank solution, any peak due to maleic acid near the start of the chromatogram and any peak with an area less than the area of the peak in the chromatogram obtained with solution (3) (0.05%).

Assay

Carry out the method for liquid chromatography, Appendix III D, using the following solutions.

(1) Add sufficient methanol to 10 whole tablets to produce a solution containing 0.02% w/v of domperidone, mix with the aid of ultrasound for 20 minutes and filter through a glass microfibre filter (Whatman GF/C is suitable). To 50 mL of the filtrate add 1 mL of 0.1m hydrochloric acid and sufficient water to produce 100 mL.
(2) 0.0127% w/v of domperidone maleate BPCRS in a mixture of equal volumes of 0.002m hydrochloric acid and methanol.
chromatographic conditions

The chromatographic procedure described under Related substances may be used.

determination of content

Calculate the content of C22H24ClN5O2 in the tablets using the declared content of C22H24ClN5O2 in domperidone maleate BPCRS.

Storage

Domperidone Tablets should be stored in an airtight container.

Labelling

The quantity of the active ingredient is stated in terms of the equivalent amount of domperidone.