高效液相色潽法测定马来酸阿法替尼对映异构体的含量

Determination of enantiomer of afatinib maleate by HPLC

目的建立测定马来酸阿法替尼对映异构体的高效液相色谱方法。方法色谱柱为CHIRALPAK IC手性柱（250 mm×4.6 mm,5μm）,以正己烷-二氯甲烷-无水乙醇-二乙胺（60∶40∶3∶0.1）为流动相,流速为0.8 m L·min-1,检测波长为250 nm,柱温为30℃,进样量10μL。结果马来酸阿法替尼及其对映异构体对照品浓度分别在0.429~5.150μg·m L-1（r=0.9997）及0.381~4.572μg·m L-1（r=0.9999）内线性关系良好;定量限浓度分别为0.286μg·m L-1、0.254μg·m L-1,检测限浓度分别为0.072μg·m L-1、0.064μg·m L-1,低、中、高3个浓度的供试品溶液平均回收率分别为99.6%、98.4%、97.6%,RSD分别为0.38%、2.4%、0.20%。结论本方法专属性强、准确度高,可用于马来酸阿法替尼对映异构体的质量控制。

ective To develop an HPLC method to determine the enantiomer of afatinib maleate. MethodsCHIRALPAK IC（250 mm×4.6 mm, 5 μm） was used with the mobile phase of n-hexane-dichloromethaneethanol-diethylamine（60∶40∶3∶0.1） at 0.8 m L·min- 1, and the detection wavelength was 250 nm. The column temperature was 30 ℃ and the injection volume was 10 μL. Results The method displayed a good linearity at 0.429- 5.150 μg·m L- 1（r = 0.9997） for afatinib maleate, and 0.381- 4.572 μg·m L- 1（r = 0.9999） for its enantiomer. The limit of quantification was 0.286 μg·m L- 1 and 0.254 μg·m L- 1, the limit of detection was 0.072 μg·m L- 1 and 0.064 μg·m L- 1, respectively. The average recovery was at 97.6%- 99.6%, with the RSD 3%. Conclusion The method is highly specific and accurate, which is suitable for the determination of enantiomer of afatinib maleate.