中国中药杂志

2008, (14) 1684-1687

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桂附地黄丸中痕量毒性成分乌头碱的限量检测
Limited determination of trace toxical aconitine alkaloid in Guifudihuang pills

李珺沬;蒋晔;
LI Jun-mei JIANG Ye (School of Pharmacy,Hebei Medical University,Shijiazhuang 050017,China)

摘要(Abstract):

目的:建立毛细管电泳场放大富集技术检测桂附地黄丸中痕量毒性成分乌头碱的方法。方法:采用未涂层熔融石英毛细管柱(50μm×43 cm,有效长度35 cm)为分离通道,50 mmol·L~(-1)磷酸二氢钠(pH 4.6)-甲醇(8:2)为运行缓冲溶液;运行电压10 kV;进样电压10 kV,进样时间40 s;在进样之前设定用甲醇冲洗,压力3.5 kPa,冲洗时间5 s;检测波长235 nm。结果:该法使乌头碱的检测灵敏度提高了500倍。乌头碱在31.3~2×10~3μg·L~(-1)呈良好的线性关系(r=0.999 6),最低检测限为9.4μg·L~(-1),平均回收率为98.0%,RSD 2.6%。结论:本方法简便、快速、专属性强、富集效率高,为桂附地黄丸的生产及质量控制提供了一种新的、可靠的分析手段。
Objective:To establish a capillary electrophoresis with field-amplified sample stacking method for the separation and determination of aconitine alkaloid in Guifudihuang pills.Method:An uncoated fused-silica capillary column(50μm×43 cm, effective length 35 cm)was used.The running buffer was 50 mmol·L~(-1)phosphate electrolyte solution(pH 4.6)-methanol(8:2). The ruuning voltage was 10 kV and the capillary inlet was dipped in methanol for 5 s prior to electrokinetic injection(10 kV,40 s). The detection wavelength was 235 nm.Result:This method allowed 500 fold enrichment of aconitine alkaloid.A good linear relation was obtained in the range of 31.3-2×10~3μg·L~(-1)(r=0.999 6),with the detection limit of 9.4μg·L~(-1).The average recovery was 98.0% with the RSD of 2.6%.Conclusion:The method is simple,rapid and specific with high stacking efficiency;it provides a new reliable means for production and quality control of Guifudihuang pills.

关键词(KeyWords): 毛细管电泳场放大富集技术;附桂地黄丸;乌头碱;限量检测
Field-amplified sample stacking capillary electrophoresis;Guifudihuang pills;aconitine alkaloid;limited determination

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作者(Author): 李珺沬;蒋晔;
LI Jun-mei JIANG Ye (School of Pharmacy,Hebei Medical University,Shijiazhuang 050017,China)

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