高效液相色谱法测定替格瑞洛原料药中异构体的含量

Determination of Isomers in Ticagrelor Bulk Drug by High Performance Liquid Chromatography

建立高效液相色谱法测定替格瑞洛原料药中异构体含量的方法。色谱柱为Phenomenex Lux Cellulose-2(250 mm×4.6 mm,5μm),流动相为无水乙醇-正己烷-异丙醇-二乙胺(体积比为55:40:5:0.5),流速为1.0 mL/min,检测波长为300 nm,柱温为20℃。在上述色谱条件下,替格瑞洛及其各异构体(DE、A、B、C)分离完全;异构体(DE、A、B、C)在相对供试品溶液浓度为0.05%~0.25%的范围内线性良好;平均回收率为92.8%~102.7%,RSD为2.2%~5.5%。本方法专属性、准确度良好,可用于替格瑞洛原料药中异构体含量的测定。

To establish a method for the determination of isomer in ticagrelor bulk drug by high performance liquid chromatography(HPLC).The chromatographic column was Phenomenex Lux Cellulose-2(250 mm×4.6 mm,5μm),the mobile phase was absolute ethanol-n-hexane-isopropanol-diethylamine(volume ratio was 55:40:5:0.5),the flow rate was 1.0 mL/min,the detection wavelength was 300 nm,and the column temperature was 20°C.Under the above chromatographic conditions,the ticagrelor and its isomers(DE,A,B,C)were separated completely.The linearity of isomers(DE,A,B,C)was good in the concentration of 0.05%~0.25%of relative tested solution,the average recovery was 92.8%~102.7%,and the RSD was 2.2%~5.5%.The method has good specificity and accuracy,and can be used for the determination of isomer in ticagrelor bulk drug.