摘要
目的:分别建立手性色谱分离法和RP-HPKC法测定左乙拉西坦右旋异构体及其他有关物质。方法:RP-HPLC法采用Inertsil C_(18)色谱柱(250 mm×4.6 mm,5μm),以乙腈-磷酸氢二钾溶液(10:90)为流动相,流速1 ml·min^(-1),检测波长205nm,柱温30℃;手性色谱分离法采用三-(3,5-二甲基苯基氨基甲酸)纤维素酯键合硅胶柱(大赛璐OD-H,250 mm×4.6 mm,5μm),以正庚烷-无水乙醇-CF_3COOH(83:17:0.1)为流动相,流速0.5 ml·min^(-1),检测波长为205 nm,柱温30℃。结果:在RP-HPLC条件下,已知杂质及破坏产生未知杂质与左乙拉西坦明显分离,左乙拉西坦最低检测限为2 ng;在手性色谱分离法条件下,左乙拉西坦与其右旋对映异构体明显分离,右旋异构体在2～10μg·ml^(-1)浓度范围内呈良好线性(r=0.999 5),方法的最低检测限为10 ng。结论:两种方法简便,灵敏,准确,可以有效检测左乙拉西坦右旋异构体及其他有关物质。
Objective：To establish a chiral chromatographic separation method and RP-HPLC method to determine R-enantiomer and the other related substances in levetiracetam.Method：An inertsil C_（18） column（250 mm×4.6 mm,5μm） with the mobile phase of acetonitrile-dipotassium hydrogenphosphate solution（10：90） was used in the RP-HPLC method.The flow rate was 1.0 ml·min^（-1）, the UV detection wavelength was set at 205 nm and the column temperature was at 30℃.A DAICEL OD-H column（250 mm×4.6 mm,5μm） with the mobile phase of n-heptane-alcohol-trifluoroacetic acid（83：17：0.1） was used in the chiral chromatographic separation method.The flow rate was 0.5 ml·min^（-1）,the UV detection wavelength was set at 205 nm and the column temperature was at 30℃.Result：Levetiracetam and its related substances could be separated well,and the lowest determination limit of levetiracetam was 2 ng in the RP-HPLC method.Levetiracetam was separated from R-enantiomer efficiently,the calibration curve of R-enantiomer was linear within the concentration range of 2-10μg·ml^（-1）（r =0.999 5） and the determination limit was 10 ng in the chiral chromatographic separation method.Conclusion：The two methods are both simple,sensitive,and accurate,and suitable for the determination of R-enantiomer and the other related substances.
出处
《中国药师》
CAS
2013年第3期331-334,共4页
China Pharmacist
基金
卫生行业科研专项(编号:200902008)
国家"十二五"重大新药创制科技重大专项(编号:2011ZX09203-001-16)
