- British Pharmacopoeia Volume III
- Formulated Preparations: Specific Monographs
Sulpiride Tablets |
Dopamine receptor antagonist; neuroleptic.
Sulpiride Tablets contain Sulpiride.
The tablets comply with the requirements stated under Tablets and with the following requirements.
95.0 to 105.0% of the stated amount.
To a quantity of the powdered tablets containing 0.2 g of Sulpiride add 20 ml of methanol, shake for 5 minutes, filter and evaporate the filtrate to dryness. The infrared absorption spectrum of the residue, Appendix II A, is concordant with the reference spectrum of sulpiride (RS 391).
A. Carry out the method for thin-layer chromatography, Appendix III A, using the following solutions.
(1) Add 20 ml of methanol to a quantity of the powdered tablets containing 0.2 g of Sulpiride, shake for 5 minutes, filter, evaporate the filtrate to dryness and dissolve the residue in 10 ml of methanol.
(2) 0.02% w/v of sulpiride impurity A EPCRS in methanol.
(3) Dilute 1 volume of solution (2) to 10 volumes with methanol.
(a) Use a silica gel HF254 precoated plate (Analtech Uniplates are suitable).
(b) Use the mobile phase as described below.
(c) Apply 10 µl of each solution.
(d) Develop the plate to 10 cm.
(e) After removal of the plate, dry in air, spray with ninhydrin solution and heat at 100° to 105° for 15 minutes.
2 volumes of 13.5m ammonia, 10 volumes of 1,4-dioxan, 14 volumes of methanol and 90 volumes of dichloromethane.
Any spot in the chromatogram obtained with solution (1) corresponding to the principal spot in the chromatogram obtained with solution (2) is not more intense than the spot in the chromatogram obtained with solution (3) (0.1%).
B. Carry out the method for liquid chromatography, Appendix III D, using the following solutions.
(1) Add 20 ml of methanol to a quantity of the powdered tablets containing 0.2 g of Sulpiride, shake for 5 minutes, filter, evaporate the filtrate to dryness and dissolve the residue in sufficient of the mobile phase to produce 200 ml.
(2) Dilute 3 volumes of solution (1) to 100 volumes with the mobile phase and dilute 1 volume of this solution to 10 volumes with the mobile phase.
(3) 0.01% w/v of sulpiride BPCRS and 0.01% w/v of sulpiride impurity B EPCRS in the mobile phase.
(a) Use a stainless steel column (25 cm × 4.6 mm) packed with octylsilyl silica gel for chromatography (5 µm) (Zorbax RX C8 is suitable).
(b) Use isocratic elution and the mobile phase described below.
(c) Use a flow rate of 1.5 ml per minute.
(d) Use an ambient column temperature.
(e) Use a detection wavelength of 240 nm.
(f) Inject 20 µl of each solution.
(g) For solution (1) and solution (2) allow the chromatography to proceed for 2.5 times the retention time of sulpiride.
10 volumes of acetonitrile, 10 volumes of methanol and 80 volumes of a solution containing 6.8% w/v of potassium dihydrogen orthophosphate and 0.1% w/v of sodium octanesulphonate, adjusted to pH 3.3 using orthophosphoric acid.
The test is not valid unless, in the chromatogram obtained with solution (3), the resolution factor between the two principal peaks is at least 2.5.
In the chromatogram obtained with solution (1):
the sum of the areas of any secondary peaks is not greater than the area of the principal peak in the chromatogram obtained with solution (2) (0.3%).
Weigh and powder 20 tablets. Mix a quantity of the powder containing 0.1 g of Sulpiride with about 50 ml of 0.1m sodium hydroxide for 5 minutes with the aid of ultrasound, add sufficient 0.1m sodium hydroxide to produce 100 ml and filter, discarding the first 10 ml of filtrate. Dilute 5 ml of the filtrate to 100 ml with 0.1m sodium hydroxide and measure the absorbance of the solution at the maximum at 291 nm, Appendix II B, using 0.1m sodium hydroxide in the reference cell. Calculate the content of C15H23N3O4S in the tablets from the absorbance of a 0.005% w/v solution of sulpiride BPCRS in 0.1m sodium hydroxide using the declared content of C15H23N3O4S in sulpiride BPCRS.
The impurities limited by the requirements of this monograph include those listed under Sulpiride.