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出 处:《中国中药杂志》2010年第24期3287-3290,共4页China Journal of Chinese Materia Medica
基 金:河北省卫生厅科研基金项目(08056)
摘 要: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17.2275,34.4550μg.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 set up a capillary electrophoresis method with field-amplified sample injection for the determination of aconitine and hypaconitine in Gucixiaotong Ye.Method: An uncoated fused-silica capillary column(50 μm×50 cm,effective length 42 cm)was used as the separation channel.The running buffer was 50 mmol·L-1 phosphate electrolyte solution(pH 9)-methanol(90∶10),the running voltage was 10 kV and the capillary inlet was dipped in methanol for 5 s prior to electrokinetic injection(12 kV,30 s),the detection wavelength was set at 235 nm.Result: Aconitine and hypaconitine were linear in the concentration ranges of 17.2-275 μg·L-1 and 34.4-550 μg·L-1,respectively.The average recovery was more than 93.9% with the RSD of 3.8%.This method could enrich 500 fold of aconitine alkaloid.Conclusion: The method is simple,rapid and specific with high stacking efficiency,it provides a new reliable means for production and quality control of Gucixiaotong Ye.
关 键 词:毛细管电泳场放大富集技术 骨刺消痛液 乌头碱 次乌头碱 限量检测
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