毛细管区带电泳法测定己烯雌酚片剂中己烯雌酚的含量

Determination of diethylstilbestrol in diethylstilbestrol tablet by capillary zone electrophoresis

目的 :用毛细管区带电泳法测定己烯雌的含量。方法 :采用 4 0cm× 5 0 μm (i.d)毛细管柱 ,以肉桂酸为内标 ,2 5mmol·L- 1硼砂 (pH =9 18)为缓冲液 ,电压 2 4kV ,虹吸进样 ,时间 1s ,紫外检测波长 2 14nm。 结果 :在 4min内可完成乙烯雌酚与内标物的分离和测定 ,最低检测限 10 0 μg·ml- 1,在 10 5 7～ 5 2 8 5 μg·ml- 1范围内线性关系良好 (r =0 9998,n =5 ) ;回收率 97 91%～ 10 1 5 8% ,日内RSD≤ 1 6 1% ,日间RSD≤3 76 %。结论 :本方法简便、快速、准确 。

OBJECTIVE:To determine the contents of diethylstilbestrol by capillary zone electroporesis(CZE).METHODS:Using cinnamon acid as the internal standard(IS),the electrophoretic separation was achieved with 25 mmol·L -1 borate(pH=9 18) as the running buffer and a voltage of 24 kV was applied to the 45cm×50μm(i.d)capillary.The analysis were introduced into capillary by siphon(1s)and determined with on column monitoring at 214nm.RESULTS:The determination could be completed within 4 min and the minimum concentration of detection was 10μg·ml -1 The analytical results of diethylstilbestrol samples demonstracted a good linear relationship within the 105.7～528.5μg·ml -1 .The relative standard deviation ( RSD )of intra-day was less than 1.61% and that of inter day was less 3.76%.The present recoveries were between 97.91%～101.58%.CONCLUSION:This method is accurate,simple,sensitive and reliable,which can be applied to the determination of diethylstilbestrol content.