高效液相色谱法测定硫酸氢氯吡格雷中的有关物质

建立高效液相色谱法测定硫酸氢氯吡格雷中的有关物质的方法。其分解产物的检测,采用SinoChrom ODS-BP（200mm×4.6mm,5μm）色谱柱,以1%（V/V）三乙胺（pH=4.0）-乙腈（25∶75）为流动相,检测波长225nm,流速1.0mL/min。硫酸氢氯吡格雷在0.48—0.72μg范围内线性关系良好（r=0.9999）,定量下限为3ng,检出限为0.6ng,各种破坏性样品的分离度符合规定。其光学纯度的测定采用ULTRON ES-OVM（Analytical）手性柱（150mm×4.6mm,5μm）,色谱填料为L57。以磷酸盐缓冲液（pH=4.67）-乙腈（75∶25）为流动相,检测波长为220nm。硫酸氢氯吡格雷相关物质B分离度均大于2.5,符合要求。本方法简便,灵敏,准确,专属性强,能够满足硫酸氢氯吡格雷对有关物质测定的要求。

Determination of Related Substances in Clopidogrel Hydrogen Sulfate by HPLC

The method for the determination of related substances in clopidogrel hydrogen sulfate was established by high performance liquid chromatography.The catabolite was detected by columnSinoChrom ODS-BP（200mm×4.6mm,5μm）] with 1%（V/V） triethylamine-acetonitrile（25∶75）as mobile phase at pH of 4.0 with a flow rate of 1.0mL/min.The detection was monitored at 225nm.The calibration curve was linear in the range of 0.48—0.72μg with the correlation coefficient of 0.9999.The limit of detection（LOQ） was 3ng.The detection limit was 0.6ng.The separation degrees of various destructive effect samples were up to specification.The optical purity was determined by ULTRON ES-OVM（analytical）chiral column（150mm×4.6mm,5μm）with packing material of L57,with phosphate buffer（pH=4.67）-acetonitrile（75∶25） as mobile phase at the detection wavelength of 220nm.The separation of related compound B of clopidogrel hydrogen sulfate was greater than 2.5.The method is simple,sensitive and accurate,that meets need for determination of related substances in clopidogrel hydrogen sulfate.