马来酸氯苯那敏BP2015翻译

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Chlorphenamine Maleate马来酸氯苯那敏General Notices总体概述(Ph. Eur. monograph 0386)C20H23ClN2O4 390.9 113-92-8Action and use使用及用途Histamine H1 receptor antagonist; antihistamine.组胺H1受体拮抗剂;抗组胺药。

Preparations制剂Chlorphenamine Injection马来酸氯苯那敏注射液Chlorphenamine Oral Solution马来酸氯苯那敏口服溶液Chlorphenamine Tablets马来酸氯苯那敏片Ph EurDEFINITION定义(3RS)-3-(4-Chlorophenyl)-N,N-dimethyl-3-(pyridin-2-yl)propan-1-amine hydrogen (Z)- butenedioate.(3RS)-3-(4-氯苯基)-N,N-二甲基-3 -(2-吡啶基)丙烷-1-胺氢(Z)—butenedioate。

Content含量98.0 per cent to 101.0 per cent (dried substance).98.0~101.0%(按干燥品计算)CHARACTERS性状Appearance外观White or almost white, crystalline powder.白色或类白色结晶性粉末Solubility溶解度Freely soluble in water, soluble in ethanol (96 per cent).易溶于水,溶于乙醇(96.0%)IDENTIFICATION鉴别A. Melting point (2.2.14): 130 °C to 135 °C.熔点(2.2.14)130℃-135℃B. Infrared absorption spectrophotometry (2.2.24).Comparison chlorphenamine maleate CRS. 红外光吸收光谱(2.2.24)与马来酸氯苯那敏的对照品一致C. Optical rotation (see Tests).旋光度(见测试)TESTS测试Solution S溶液澄清度与颜色(溶液S)Dissolve 2.0 g in water R and dilute to 20.0 mL with the same solvent.取供试品2.0g,置于20ml容量瓶中,用水溶解并稀释至刻度。

Appearance of solution溶液外观Solution S is clear (2.2.1) and not more intensely coloured than reference solution BY6(2.2.2, Method II).溶液S应澄清无色;如显色,与BY6比较不得更深。

Optical rotation (2.2.7)旋光度-0.10° to + 0.10°, determined on solution S.-0.10°-+0.10°,用溶液S测定Related substances有关物质Liquid chromatography (2.2.29).高效液相色谱法(2.2.29)Test solution Dissolve 0.100 g of the substance to be examined in the mobile phase and dilute to 100.0 mL with the mobile phase.供试品溶液:精密称取供试品0.100g,置100ml容量瓶中,用流动相溶解并定量稀释至刻度,即得。

Reference solution (a) Dilute 0.5 mL of the test solution to 100.0 mL with the mobilephase.对照溶液a:精密量取供试品溶液0.5ml置100ml容量瓶中,用流动相定量并稀释至刻度,即得。

Reference solution (b) Dilute 1.0 mL of reference solution (a) to 10.0 mL with the mobile phase.对照溶液b:精密量取对照溶液a1.0ml,置10ml容量瓶中,用流动相定量并稀释至刻度,即得。

Reference solution (c) Dissolve 5 mg of chlorphenamine impurity C CRS in 5 mL of the test solution and dilute to 50.0 mL with the mobile phase. Dilute 2 mL of this solutionto 20 mL with the mobile phase.对照溶液c:精密量取杂质C 对照品5mg,置50.0ml容量瓶中,用5ml的供试品溶液溶解,加入流动相溶解并稀释至刻度,摇匀。

再取该溶液2ml置20ml容量瓶中,并用流动相溶解并稀释至刻度,即得。

Reference solution (d) Dissolve 5 mg of 2,2¢-dipyridylamine R (impurity B) in the mobile phase and dilute to 100 mL with the mobile phase.对照溶液d:精密量取5mg的杂质B 置100ml的容量瓶中,用流动相溶解并定量稀释至刻度即得。

Reference solution (e) Dissolve the contents of a vial of chlorphenamine impurity A CRS in 2 mL of the test solution. Sonicate for 5 min.对照溶液e:精密量取含有杂质A的对照品,用2ml的供试品溶液溶解,超声5分钟。

Column:柱—size: l = 0.30 m, Ø = 3.9 mm;尺寸—stationary phase: octadecylsilyl silica gel for chromatography R (10 μm).固定相:十八烷基硅胶色谱(10μm)Mobile phase Mix 20 volumes of acetonitrile R and 80 volumes of a 8.57 g/L solution of ammonium dihydrogen phosphate R previously adjusted to pH 3.0 with phosphoric acid R.流动相:乙腈-磷酸二氢铵溶液8.57g/L(事先用磷酸调节pH至3.0)(20:80)Flow rate 1.2 mL/min.流速:1.2ml/minDetection Spectrophotometer at 225 nm.分光光度计检测波长225nmInjection 20 μL.进样体积20μlRun time 3.5 times the retention time of chlorphenamine.运行时间为氯苯那敏保留时间的3.5倍Relative retention 相对保留时间With reference to chlorphenamine (retention time = about 11 min):maleic acid = about 0.2;impurity A = about 0.3;impurity B = about 0.4;impurity C = about 0.9;impurity D = about 3.0.马来酸约0.2;杂质A约0.3;杂质B= 0.4;杂质C约0.9;杂质D约3.0。

System suitability: reference solution (c):—resolution: minimum 1.5 between the peaks due to impurity C and chlorphenamine.系统适用性溶液(对照溶液c)分辨率:杂质C和氯苯那敏色谱峰之间的分离度应大于1.5Limits:限度—correction factors: for the calculation of contents, multiply the peak areas of the following impurities by the corresponding correction factor: impurity A = 1.5; impurity B= 1.4;校正因子:对于含量的计算,通过以下杂质的峰面积乘以相应的校正因子:杂质A= 1.5;杂质B= 1.4;—impurity A: not more than 0.4 times the area of the principal peak in the chromatogram obtained with reference solution (a) (0.2 per cent);杂质A:不得大于对照溶液a所得图谱中主峰面积的0.4倍(0.2%)—impurities B, C, D: for each impurity, not more than 0.2 times the area of the principal peak in the chromatogram obtained with reference solution (a) (0.1 per cent);杂质B、C、D:任一杂质,不得大于对照溶液a所得图谱中主峰面积的0.2倍(0.1%) —unspecified impurities: for each impurity, not more than 0.2 times the area of the principal peak in the chromatogram obtained with reference solution (a) (0.10 percent);其他杂质:不得大于对照溶液a所得图谱中主峰面积的0.2倍—total: not more than the area of the principal peak in the chromatogram obtained with reference solution (a) (0.5 per cent);总杂质:不得大于对照溶液a得到的主峰面积(0.5%)—disregard limit: the area of the principal peak in the chromatogram obtained with reference solution (b) (0.05 per cent); disregard the peaks due to the blank and maleic acid.在色谱图中由溶液b得到的色谱峰面积(0.05%)可忽略不及;空白和马来酸的峰可忽略不计。