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目的建立毛细管电泳场放大富集技术快速检测温胃舒颗粒中痕量有效毒性成分乌头碱的方法。方法采用未涂层石英毛细管(43cm×50μm,有效长度35cm)为分离通道,60mmol/L磷酸二氢钠(pH6.0)-乙腈(8:2)为运行缓冲溶液;运行电压10kV;进样电压12kV,进样时间30s;在进样之前设定用水冲洗,压力为3.5kPa,冲洗时间5s;紫外检测波长235nm。结果乌头碱在37.5~2.4×103ng/mL线性关系良好(r=0.9995),最低检测限为11.3ng/mL,平均回收率大于97.3%。结论本方法简便、快速、专属性强、富集效率高,为温胃舒颗粒在生产过程中的质量控制及临床药物监测提供可靠的分析手段。
Objective To establish a capillary electrophoresis field amplification and enrichment technique for the rapid detection of aconitine, a trace of effective toxic components in Wenweishu granules. Methods Uncoated quartz capillary (43cm×50μm, effective length: 35cm) was used as the separation channel. 60mmol/L sodium dihydrogen phosphate (pH6.0)-acetonitrile (8:2) was used as running buffer solution; operating voltage was 10kV; Voltage 12kV, injection time 30s; set flush with water before injection, pressure is 3.5kPa, rinse time 5s; UV detection wavelength 235nm. Results The aconitine had a good linear relationship (r=0.9995) at 37.5~2.4×10 3 ng/mL. The detection limit was 11.3 ng/mL. The average recovery rate was greater than 97.3%. Conclusion This method is simple, rapid, specific and high enrichment efficiency. It provides a reliable analytical method for the quality control and clinical drug monitoring of Wenweishu Granules in the production process.