摘要:
目的 用毛细管区带电泳法测定己烯雌的含量。方法 采用 40cm× 50μm (i.d)毛细管柱,以肉桂酸为内标,25mmol·L-1硼砂 (pH=9.18)为缓冲液,电压 24kV,虹吸进样,时间 1s,紫外检测波长 214nm. 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 10.0μg·ml-1,在 105.7～528.5μg·ml-1范围内线性关系良好 (r=0.9998,n=5);回收率 97.91%～101.58%,日内RSD≤ 1.61%,日间RSD≤3.76%.结论 本方法简便、快速、准确,适用于该制剂的质量控制。
Abstract:
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-1borate(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 w ithin 4 min and the minimum concentration of detection was 10μg·ml-1.The analytical results of diethylstilbestrol samples demonstraoted 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 bettween 97.91%-101.58%.CONCLUSION This method is accurate, simple, sensitive and reliable, which can be applied to the determination of diethylstilbestrol content.
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