毛细管电泳法对肝素钠注射液中杂质的测定

目的: 在2008年国家食品药品监督管理局颁布的"毛细管电泳法分析肝素钠杂质的补充检验方法"的基础上优化毛细管电泳色谱条件,对全国评价性抽验肝素钠注射液样品进行测定。 方法: 采用毛细管电泳法,缓冲液为pH 3.0的400 mmol·L^-1三羟甲基氨基甲烷(Tris)溶液;分离电压为-25 kV;检测波长为200 nm;进样压力3.447 kPa,进样时间为4 s;毛细管温度:25 ℃。 结果: 肝素主峰与多硫酸软骨素峰峰之间分离度为1.0,与硫酸皮肤素之间分离度为2.0,10批供试品的杂质含量结果与离子色谱法结果基本一致。 结论: 优化后的色谱条件使肝素与硫酸皮肤素、多硫酸软骨素的分离度增加,该方法使肝素钠样品中的杂质定性、定量更为准确。

Objective: In 2008,the Heparin Sodium impurities test method employing capillary electrophoresis(CE) was introduced by the State Food and Drug Administration(SFDA).As the poor separation between the impurities and the heparin,we proposed to optimize the method,and used it to test the contaminants of 10 batches of heparin sodium injection for the national drug assessment. Methods: CE-UV method was used,BGE,400 mmol·L^-1 Tris solution;Voltage,-25 kV;detection wavelength,200 nm;sample injection,4 s at 3.447 kPa;capillary temperature,25 ℃. Results: The oversulfated chondroitin sulfate(OSCS)-heparin resolution was 1.0,while the heparin-dermatan sulfate(DS) resolution was 2.0,and the impurity contents of the samples were consist to the ion chromatography(IC) results. Conclusions: Enhancement of the OSCS-heparin and heparin-DS separation was achieved,and this method is reliable for the quantitative and quantitative analysis of heparin.