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目的:建立毛细管电泳场放大富集技术测定骨刺消痛液中乌头碱类痕量毒性成分的方法。方法:采用未涂层石英毛细管(50μm×50 cm,有效长度42 cm)为分离通道,50 mmol.L-1磷酸二氢钠(pH9)-乙腈(90∶10)为运行缓冲溶液;进样电压12 kV,进样时间30 s;在进样之前设定用水冲洗,压力3.5 kPa,冲洗时间5 s;运行电压10 kV;紫外检测波长235 nm。结果:乌头碱、次乌头碱分别在17.2~275,34.4~550μg.L-1,线性关系良好,回收率大于93.9%,RSD小于3.8%,富集倍数达到500倍。结论:本法操作简便,灵敏度高,专属性强,富集倍数高,为骨刺消痛液中乌头碱类生物碱的限量检测提供一种新型的分析手段。
OBJECTIVE: To establish a method for the determination of aconitine trace toxic components in Guchi Xiao pain fluid by capillary electrophoresis enrichment technology. Methods: Uncoated quartz capillary (50 μm × 50 cm, effective length 42 cm) was used as the separation channel and 50 mmol·L-1 sodium phosphate monobasic (pH9) -acetonitrile (90:10) Voltage 12 kV, injection time 30 s; set water flush before injection, pressure 3.5 kPa, rinsing time 5 s; operating voltage 10 kV; UV detection wavelength 235 nm. Results: Aconitine and hypaconitine showed good linearity with the recovery of more than 93.9%, RSD less than 3.8%, and enrichment multiple of 500 times, respectively, at 17.2-275.34.4-550μg.L-1. Conclusion: The method is simple, sensitive, specific, and high enrichment factor. It provides a new analytical method for the limited detection of aconitine alkaloids in Spurge Pain fluid.