Hyoscine Tablets

General Notices

Action and use

Anticholinergic.

Definition

Hyoscine Tablets contain Hyoscine Hydrobromide.

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

Content of hyoscine hydrobromide, C17H21NO4,HBr,3H2O

90.0 to 110.0% of the stated amount.

Identification

A. Carry out the method for thin-layer chromatography, Appendix III A, using the following solutions.
(1) Shake a quantity of powdered tablets containing 0.5 mg of Hyoscine Hydrobromide with 5 mL of 0.1m hydrochloric acid. Mix, with gentle swirling, with three 5-mL quantities of dichloromethane discarding the dichloromethane layers. Add 1 mL of 5m ammonia to the aqueous phase and extract with two 5-mL quantities of dichloromethane and retain the dichloromethane extracts. Dry the combined dichloromethane extracts over anhydrous sodium sulfate, filter, evaporate the filtrate to dryness and dissolve the residue in 0.5 mL of ethanol (96%).
(2) 0.1% w/v of hyoscine hydrobromide BPCRS in ethanol (96%).
chromatographic conditions
(a) Use as the coating silica gel for chromatography (Merck 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, heat it at 105° for 20 minutes, allow to cool and spray with potassium iodobismuthate solution R1.
mobile phase

10 volumes of diethylamine, 40 volumes of acetone and 50 volumes of dichloromethane.

confirmation

The principal spot in the chromatogram obtained with solution (1) corresponds in position and colour to that in the chromatogram obtained with solution (2).

B. In the test for Uniformity of content, the chromatogram obtained with solution (1) shows a peak with the same retention time as the principal peak in the chromatogram obtained with solution (2).

Tests

Uniformity of content

Tablets containing less than 2 mg and/or less than 2% w/w of Hyoscine Hydrobromide comply with the requirements stated under Tablets using the following method of analysis. Carry out the method for liquid chromatography, Appendix III D, using the following solutions. Solution A is a 0.02% w/v solution of atropine sulfate BPCRS (internal standard) in a mixture of 25 volumes of acetonitrile and 75 volumes of water.

(1) Add 1 mL of solution A to one tablet and disintegrate with the aid of ultrasound. Shake the mixture for 2 minutes, centrifuge and filter the supernatant liquid using a suitable 0.45-µm filter.
(2) 0.015% w/v of hyoscine hydrobromide BPCRS in solution A.
chromatographic conditions
(a) Use a stainless steel column (20 cm × 4.6 mm) packed with octadecylsilyl silica gel for chromatography (10 µm) (Lichrosorb RP18 is suitable).
(b) Use isocratic elution and the mobile phase described below.
(c) Use a flow rate of 2 mL per minute.
(d) Use an ambient column temperature.
(e) Use a detection wavelength of 240 nm.
(f) Inject 20 µL of each solution.
mobile phase

0.05m sodium octanesulfonate in a mixture of 1 volume of a 60% w/v solution of perchloric acid, 3 volumes of methanol, 21 volumes of acetonitrile and 75 volumes of water.

determination of content

Calculate the content of C17H21NO4,HBr,3H2O in each tablet using the declared content of C17H21NO4,HBr in hyoscine hydrobromide BPCRS. Each mg of C17H21NO4,HBr is equivalent to 1.141 mg of C17H21NO4,HBr,3H2O.

Assay

Carry out the method for liquid chromatography, Appendix III D, using the following solutions. Solution A is a 0.02% w/v solution of atropine sulfate BPCRS (internal standard) in a mixture of 25 volumes of acetonitrile and 75 volumes of water.

(1) Add to 10 whole tablets 7 mL of acetonitrile (25%), disintegrate with the aid of ultrasound and shake the mixture for 2 minutes. Add sufficient of a mixture of 25 volumes of acetonitrile and 75 volumes of water to produce a final solution containing 0.015% w/v of Hyoscine Hydrobromide, centrifuge and filter the supernatant liquid using a suitable 0.45-µm filter.
(2) Prepare solution (2) in the same manner as solution (1) but using solution A in place of a mixture of 25 volumes of acetonitrile and 75 volumes of water.
(3) 0.015% w/v of hyoscine hydrobromide BPCRS in solution A.
chromatographic conditions

The chromatographic conditions described under Uniformity of content may be used.

determination of content

Calculate the content of C17H21NO4,HBr,3H2O in the tablets using the declared content of C17H21NO4,HBr in hyoscine hydrobromide BPCRS. Each mg of C17H21NO4,HBr is equivalent to 1.141 mg of C17H21NO4,HBr,3H2O.