- British Pharmacopoeia Volume III
- Formulated Preparations: Specific Monographs
Hyoscine Butylbromide Tablets |
Anticholinergic.
Hyoscine Butylbromide Tablets contain Hyoscine Butylbromide.
The tablets comply with the requirements stated under Tablets and with the following requirements.
92.5 to 107.5% of the stated amount.
A. Shake a quantity of the powdered tablets containing 50 mg of Hyoscine Butylbromide with 20 mL of chloroform, filter, evaporate the filtrate to dryness and triturate the residue with 5 mL of acetonitrile. Evaporate to dryness and dry the residue at 50° at a pressure not exceeding 0.7 kPa for 1 hour. The infrared absorption spectrum of the residue, Appendix II A, is concordant with the reference spectrum of hyoscine butylbromide (RS 185).
B. To 1 mg of the residue obtained in test A add 0.2 mL of fuming nitric acid and evaporate to dryness on a water bath. Dissolve the residue in 2 mL of acetone and add 0.1 mL of a 3% w/v solution of potassium hydroxide in methanol. A violet colour is produced.
C. Shake a quantity of the powdered tablets containing 50 mg of Hyoscine Butylbromide with 20 mL of chloroform, filter, evaporate the filtrate to dryness, shake the residue with 50 mL of water and filter. The light absorption of the filtrate, Appendix II B, in the range 230 to 350 nm exhibits maxima at 252, 257 and 264 nm and a less well-defined maximum at 247 nm.
Carry out the method for liquid chromatography, Appendix III D, using the following solutions.
(1) Shake a quantity of the powdered tablets containing 0.1 g of Hyoscine Butylbromide with 10 mL of 0.001m hydrochloric acid with the aid of ultrasound for 15 minutes, centrifuge and filter.
(2) 0.0010% w/v of hyoscine hydrobromide BPCRS in 0.001m hydrochloric acid.
(3) Add 10 µL of solution (1) to 10 mL of solution (2).
(a) Use a stainless steel column (25 cm × 4.6 mm) packed with octylsilyl silica gel for chromatography (10 µm) (Lichrosorb 10µ C8 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 210 nm.
(f) Inject 20 µL of each solution.
2.0 g of sodium dodecyl sulfate in a mixture of 370 mL of 0.001m hydrochloric acid and 680 mL of methanol.
The test is not valid unless the resolution factor between the peaks corresponding to hyoscine and butylhyoscine is at least 5.
In the chromatogram obtained with solution (1):
the area of any peak corresponding to hyoscine is not greater than the area of the principal peak in the chromatogram obtained with solution (2) (0.1%).
Carry out the method for thin-layer chromatography, Appendix III A, using the following solutions in 0.01m hydrochloric acid.
(1) Shake a quantity of the powdered tablets containing 20 mg of Hyoscine Butylbromide with 5 mL of 0.01m hydrochloric acid and centrifuge.
(2) Dilute 3 volumes of solution (1) to 100 volumes.
(3) Dilute 1 volume of solution (1) to 50 volumes.
(4) Dilute 1 volume of solution (1) to 400 volumes.
(a) Use a silica gel F254 high-performance precoated plate (Merck silica gel 60 F254 HPTLC plates are suitable).
(b) Use the mobile phase as described below.
(c) Apply 2 µL of each solution.
(d) Develop the plate to 4 cm.
(e) After removal of the plate, dry it at 60° for 15 minutes, spray with a solution prepared by mixing equal volumes of a 40% w/v solution of potassium iodide in water and a solution prepared by dissolving 0.85 g of bismuth oxynitrate in a mixture of 10 mL of glacial acetic acid and 40 mL of water and diluting 1 volume of the mixture with 2 volumes of glacial acetic acid and 10 volumes of water immediately before use. Allow the plate to dry in air, spray well with a 5% w/v solution of sodium nitrite and examine immediately.
0.5 volumes of anhydrous formic acid, 1.5 volumes of water, 9 volumes of absolute ethanol and 9 volumes of dichloromethane.
In the chromatogram obtained with solution (1) the principal spot has an Rf value of about 0.45.
In the chromatogram obtained with solution (1):
any secondary spot with an Rf value less than that of the principal spot is not more intense than the spot in the chromatogram obtained with solution (2) (3%);
not more than two such spots are more intense than the spot in the chromatogram obtained with solution (4) (0.25%);
any secondary spot with an Rf value greater than that of the principal spot is not more intense than the spot in the chromatogram obtained with solution (3) (2%);
not more than one such spot is more intense than the spot in the chromatogram obtained with solution (4) (0.25%).
Weigh and powder 20 tablets. Carry out the method for liquid chromatography, Appendix III D, using the following solutions in 0.001m hydrochloric acid.
(1) Shake a quantity of the powdered tablets containing 40 mg of Hyoscine Butylbromide with 60 mL of the solvent with the aid of ultrasound for 15 minutes, dilute to 100 mL with the same solvent, centrifuge and filter to obtain a clear filtrate.
(2) 0.04% w/v of hyoscine butylbromide BPCRS.
The chromatographic conditions described under the test for Hyoscine may be used.
Calculate the content of C21H30BrNO4 in the tablets using the declared content of C21H30BrNO4 in hyoscine butylbromide BPCRS.