HPLC法同时测定卡非佐米中3种手性异构体含量

Simultaneous Determination of 3 Optical Isomers in Carfilzomib by HPLC

目的:建立了HPLC法直接检测卡非佐米光学异构体的方法。方法:采用Chiralpak OX-H手性柱,以正己烷-异丙醇-乙醇(89∶5∶6,v/v/v)为流动相,流速为1.0 ml·min^(-1),检测波长为220 nm。结果:对映异构体、非对映异构体Ⅰ、非对映异构体Ⅱ分别在0.54~2.14μg·ml^(-1),0.11~1.80μg·ml^(-1),0.11~1.81μg·ml^(-1)范围内线性关系良好(r≥0.998);检出限为0.07~0.27μg·ml^(-1),回收率为99.6%~100.9%,RSD为1.13%~1.59%(n=9)。结论:该方法灵敏、简便、快速、准确、特异性良好,可作为卡非佐米中对映异构体和非对映异构体杂质限量的控制方法。

Objective： To establish an HPLC method for the determination of optical isomers in carfilzomib. Methods： The sample was separated on a Chiralpak OX-H column. The mobile phase consisted of n-hexane： isopropanot： alcohol （89：5：6, v/v/v） with a flow rat of 1.0 ml μg·ml-1. The detection wavelength was 220 nm. Results： The linear rang of enantiomer, diastereomer I and di- astereomer Ⅱ was 0.54-2.14 μg·ml-1,0.11-1.80 μg·ml-1 and 0.11-1.81 μg·ml-1 （r≥0. 998）, respectively. The lower limit of quantification was 0.07-0.27 μg·ml-1. The recoveries of optical isomers were within the range of 99.6%-100.9% with RSD of 1.13% -1.59% （ n = 9）. Conclusion ： The method is sensitive, simple, fast, accurate and specific, and suitable for the study of opti- cal isomers in carfilzomib.