佐匹克隆原料BP标准.pdf

British Pharmacopoeia Volume I II Monographs: Medicinal and Pharmaceutical Substances Zopiclone General Notices (Ph Eur monograph 1060) C H ClN O 388.8 43200-80-2 17 17 6 3 Action and use Non-benzodiazepine hypnotic. Preparation Zopiclone Tablets Ph Eur DEFINITION (5RS)-6-(5-Chloropyridin-2-yl)-7-oxo-6,7-dihydro-5H-pyrrolo[3,4-b]pyrazin-5-yl 4-methylpiperazine-1-carboxylate. Content 98.5 per cent to 100.5 per cent. CHARACTERS Appearance White or slightly yellowish powder. Solubility Practically insoluble in water, freely soluble in methylene chloride, sparingly soluble in acetone, practically insoluble in ethanol (96 per cent). It dissolves in dilute mineral acids. mp: about 177 °C, with decomposition. IDENTIFICATION First identification B. Second identification A, C. A. Ultraviolet and visible absorption spectrophotometry (2.2.25). Test solution Dissolve 50.0 mg in a 3.5 g/l solution of hydrochloric acid R and dilute to 100.0 ml with the same solvent. Dilute 2.0 ml of this solution to 100.0 ml with a 3.5 g/l solution of hydrochloric acid R. Spectral range 220-350 nm. Absorption maximum At 303 nm. Specific absorbance at the absorption maximum 340 to 380. B. Infrared absorption spectrophotometry (2.2.24). Preparation Discs. Comparison zopiclone CRS. C. Thin-layer chromatography (2.2.27). Test solution Dissolve 10 mg of the substance to be examined in methylene chloride R and dilute to 10 ml with the same solvent. Reference solution Dissolve 10 mg of zopiclone CRS in methylene chloride R and dilute to 10 ml with the same solvent. Plate TLC silica gel GF254 plate R. Mobile phase triethylamine R, acetone R, ethyl acetate R (2:50:50 V/V/V). Application 10 µl. Development Over a path of 15 cm. Drying In air. Detection Examine in ultraviolet light at 254 nm. Results The principal spot in the chromatogram obtained with the test solution is similar in position and s