高效液相色谱法测定泊沙康唑甲苯磺酸酯的对映异构体杂质

Determination of Enantiomeric Impurities of Posaconazole Toluene Sulfonate by High Performance Liquid Chromatography

建立高效液相色谱法测定泊沙康唑关键起始物料泊沙康唑甲苯磺酸酯的对映异构体杂质,该方法使用表面共价键合有直链淀粉-三(3,5-二甲基苯基氨基甲酸酯)硅胶为填充剂的色谱柱(大赛璐CHIRALPAK IA,250 mm×4.6 mm,5μm),流动相为正己烷-无水乙醇(65:35),流速为1.0 mL/min,柱温为30℃,波长为225 nm,进样体积为10μL。对映异构体杂质的定量限为0.3μg/mL,在0.3~2.0μg/mL范围内的线性关系良好,平均回收率为98.5%,回收率RSD为0.8%。本方法专属性和准确度良好,灵敏度较高,可用于泊沙康唑甲苯磺酸酯的质量控制。

A high performance liquid chromatography(HPLC)method has been established for detecting the enantiomer impurity of posaconazole toluene sulfonate,a key starting material of posaconazole.A Daicel CHIRALPAK IA column(250 mm×4.6mm,5μm)was used,with the mobile phase of N-hexane-anhydrous ethanol(65:35),flow rate was 1.0 mL/min,the column temperature was set at 30℃,the wavelength of detector was 225 nm,and the injection volume was 10μL.The limit of quantitation of the enantiomer impurity was 0.3μg/mL,the method was linear from 0.3μg/mL to 2.0μg/mL,the accuracy was similar with a mean(RSD)ratio of 98.5%(0.8%).The method is simple,specific and sensitive,and can be used for the quality control of Posaconazole toluene sulfonate.