Edition: BP 2025 (Ph. Eur. 11.6 update)
General Notices
Action and use
Anticholinergic.
DEFINITION
Hyoscine Butylbromide Injection is a sterile solution of Hyoscine Butylbromide in Water for Injections.
The injection complies with the requirements stated under Parenteral Preparations and with the following requirements.
Content of hyoscine butylbromide, C21H30BrNO4
95.0 to 105.0% of the stated amount.
IDENTIFICATION
A. Evaporate to dryness a volume containing 0.1 g of Hyoscine Butylbromide, shake the residue with 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. In the Assay, 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
Acidity
pH, 3.7 to 5.5, Appendix V L.
Related substances
Carry out the method for liquid chromatography, Appendix III D, using the following solutions.
(1) Dilute a quantity of the injection containing 100 mg of Hyoscine Butylbromide to 20 mL with 0.001M hydrochloric acid.
(2) Dilute 1 volume of solution (1) to 50 volumes with 0.001M hydrochloric acid, further dilute 1 volume of this solution to
10 volumes with the same solvent.
(3) 0.006% w/v of tropic acid (impurity B) in 0.001M hydrochloric acid.
(4) 0.5% w/v of hyoscine butylbromide BPCRS and 0.003% w/v of tropic acid in 0.001M hydrochloric acid.
CHROMATOGRAPHIC CONDITIONS
(a) Use a stainless steel column (12.5 cm × 4 mm) packed with base-deactivated end-capped octylsilyl silica gel for chromatography (5 μm) (LiChrospher 60 RP-select B 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 a column temperature of 45°.
(e) Use a detection wavelength of 220 nm.
(f) Inject 10 μL of each solution.
MOBILE PHASE
Solution A a mixture containing 1.265% w/v of sodium dihydrogen orthophosphate monohydrate and 0.34% w/v of tetrabutylammonium hydrogen sulfate, adjust the pH to 5.5 with 0.5M sodium hydroxide as necessary. 125 volumes of methanol and 875 volumes of solution A.
When the chromatograms are recorded under the prescribed conditions, the relative retentions with reference to hyoscine butylbromide (retention time about 5 minutes) are: tropic acid (impurity B), about 1.3 and impurity G, about 2.6.
SYSTEM SUITABILITY
The test is not valid unless, in the chromatogram obtained with solution (4), the resolution between the peaks due to hyoscine butylbromide and tropic acid is at least 1.5.
LIMITS
In the chromatogram obtained with solution (1):
Identify any peak due to impurity G using the specified retention time and multiply the area of the peak by the correction factor of 0.41; the area of any peak corresponding to tropic acid is not greater than the area of the principal peak in the chromatogram obtained with solution (3) (1.2%);
the area of any peak corresponding to impurity G is not greater than 5 times the area of the principal peak in the chromatogram obtained with solution (2) (1%);
the area of any other secondary peak is not greater than the area of the principle peak in the chromatogram obtained with solution (2) (0.2%);
the sum of the impurities is not greater than 2.5%.
Disregard any peak with an area less than half the area of the principal peak in the chromatogram obtained with solution
(2) (0.1%).
ASSAY
Carry out the method for liquid chromatography, Appendix III D, using the following solutions.
(1) Dilute a quantity of the injection containing 100 mg of Hyoscine Butylbromide to 20 mL with 0.001M hydrochloric acid.
(2) 0.5% w/v of hyoscine butylbromide BPCRS in 0.001M hydrochloric acid.
(3) 0.5% w/v of hyoscine butylbromide BPCRS and 0.003% w/v of tropic acid in 0.001M hydrochloric acid.
CHROMATOGRAPHIC CONDITIONS
The chromatographic conditions described under Related substances may be used.
DETERMINATION OF CONTENT
Calculate the content of C21H30BrNO4 in the injection using the declared content of C21H30BrNO4 in hyoscine butylbromide BPCRS.
STORAGE
Hyoscine Butylbromide Injection should be protected from light.
IMPURITIES
The impurities limited by the requirements of this monograph include impurities A, B and G listed under Hyoscine Butylbromide.
