食品科学

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高效液相色谱-串联质谱法同时测定中草药饮料中11 种有毒生物碱

马晓斐1,梁天佐1,宋 炜2,冯浩彬1,张 岩1,*   

  1. 1.河北省食品质量监督检验研究院,河北 石家庄 050091;2.河北省食品药品检验院,河北 石家庄 050011
  • 出版日期:2014-04-25 发布日期:2014-05-13
  • 通讯作者: 张 岩
  • 基金资助:

    河北省科学技术研究与发展计划项目(12277122D)

Simultaneous Determination of 11 Poisonous Alkaloids in Chinese Medicinal Herbal Beverages by Liquid Chromatography Tandem Mass Spectrometry

MA Xiao-fei1, LIANG Tian-zuo1, SONG Wei2, FENG Hao-bin1, ZHANG Yan1,*   

  1. 1. Hebei Institute of Food Quality Supervision Inspection and Research, Shijiazhuang 050091, China;
    2. Hebei Provincial Institute for Food and Drug Control, Shijiazhuang 050011, China
  • Online:2014-04-25 Published:2014-05-13
  • Contact: ZHANG Yan

摘要:

建立同时测定中草药饮料中11 种有毒生物碱(乌头碱、次乌头碱、新乌头碱、马钱子碱、士的宁、秋水 仙碱、喜树碱、阿托品、东莨菪碱、毛果芸香碱和鬼臼毒素)的高效液相色谱-串联质谱分析方法。试样直接过 0.22 μm滤膜,经Kinetex C18色谱柱(2.1 mm×100 mm,2.6 μm)分离后,在多反应监测模式下定性及定量分析。结 果表明:11 种有毒生物碱在在其线性范围内与其峰面积线性关系良好(>0.999 0),方法检出限为0.05~0.5 μg/L, 在低、中、高3 个添加水平范围内的平均回收率为75.0%~88.4%,相对标准偏差均小于7.6%。该方法操作简便、灵 敏度高、重复性好、定性定量准确,适用于中草药饮料中有毒生物碱的测定。

关键词: 饮料, 高效液相色谱, 质谱, 有毒生物碱

Abstract:

A method for the simultaneous determination of 11 poisonous alkaloids (aconitine, hypaconitine, mesaconitine, brucine,
strychnine, colchicine, camptothecin, atropine, scopolamine, pilocarpine, and podophyllotoxin) in Chinese medicinal herbal
beverages was developed by liquid chromatography tandem mass spectrometry (LC-MS-MS). Samples were filtered through a
0.22 μm microporous membrane. Qualitative and quantitative analyses were carried out by mass spectrometry under the MRM
mode after the chromatographic separation on a Kinetex C18 (2.1 mm × 100 mm, 2.6 μm) column. All the 11 poisonous alkaloids
showed a good linearity with correlation coefficients (r) no less than 0.999 0 within their linear ranges. The limits of detection for
these poisonous alkaloids were in the range of 0.05 to 0.5 μg/kg. The mean recoveries at three spiked levels were 75.0%–88.4%
and the relative standard deviations were less than 7.6%. This method is simple, sensitive, accurate and suitable for the
simultaneous analysis of poisonous alkaloids in Chinese medicinal herbal beverages.

Key words: beverage, liquid chromatography, mass spectrometry, poisonous alkaloids

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