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目的建立毛细管电泳场放大富集技术同时检测骨筋丸胶囊中有效毒性成分士的宁和马钱子碱的方法。方法选择未涂渍弹性石英毛细管(50μm×57 cm,有效分离长度50 cm)为分离通道,20 mmol/L醋酸钠(醋酸调pH3.8)为运行缓冲溶液;运行电压20 kV;进样电压20 kV,进样时间25 s;在进样之前设定用水冲洗,压力为3.5 kPa,冲洗时间3 s;紫外检测波长260 nm。结果该方法使士的宁和马钱子碱的检测灵敏度分别提高了600倍和400倍。士的宁在14.8~940.0μg/L浓度范围内线性关系良好(r=0.999 8),最低检测限为1.48μg/L,平均回收率为98.5%,RSD为1.9%;马钱子碱在17.2~1090.0μg/L浓度范围内线性关系良好(r=0.999 9),最低检测限为2.58μg/L,平均回收率为98.5%,RSD为1.8%。结论本方法简便、快速、富集效率高,为骨筋丸胶囊生产过程中的质量控制及临床药物监测提供了一种新的、可靠的分析手段。
Objective To establish a capillary electrophoresis field amplification and enrichment technique for the simultaneous determination of strychnine and strychnine, the effective toxic components in Gujin Pill Capsule. Methods The uncoated elastic quartz capillary (50 μm×57 cm, effective separation length 50 cm) was selected as the separation channel, 20 mmol/L sodium acetate (acetic acid pH 3.8) was used as the running buffer solution; the operating voltage was 20 kV; injection voltage 20 kV, injection time 25 s; set flush with water before injection, pressure 3.5 kPa, rinse time 3 s; UV detection wavelength 260 nm. Results The method improved the detection sensitivity of strychnine and strychnine by 600 and 400 times, respectively. Shih-ning has a good linearity in the concentration range of 14.8~940.0μg/L (r=0.999 8), the lowest detection limit is 1.48μg/L, the average recovery rate is 98.5%, RSD is 1.9%, and brucine is 17.2. The linearity was good in the range of ~1090.0μg/L (r=0.999 9), the detection limit was 2.58μg/L, the average recovery was 98.5%, and the RSD was 1.8%. Conclusion This method is simple, rapid, and has high enrichment efficiency. It provides a new and reliable analytical method for quality control and clinical drug monitoring in the production process of Gujin Pill Capsule.