色谱

色谱 ›› 2013, Vol. 31 ›› Issue (7): 709-713.DOI: 10.3724/SP.J.1123.2012.12025

• 研究论文 • 上一篇    下一篇

高效液相色谱-串联质谱法测定保健食品中的23种精神药品

朱琳1, 阮丽萍2, 刘华良2, 吉文亮2, 马永建1,2   

  1. 1. 东南大学公共卫生学院, 江苏 南京 210009;
    2. 江苏省疾病预防与控制中心, 江苏 南京 210009
  • 收稿日期:2012-12-19 修回日期:2013-03-11 出版日期:2013-07-28 发布日期:2013-07-17
  • 通讯作者: 马永建
  • 基金资助:

    江苏省科技厅科技支撑计划项目(BE2010745).

Simultaneous determination of 23 sedative drugs in health foods by high performance liquid chromatography-tandem mass spectrometry

ZHU Lin1, RUAN Liping2, LIU Hualiang2, JI Wenliang2, MA Yongjian1,2   

  1. 1. School of Public Health, Southeast University, Nanjing 210009, China;
    2. Jiangsu Provincial Center for Disease Control and Prevention, Nanjing 210009, China
  • Received:2012-12-19 Revised:2013-03-11 Online:2013-07-28 Published:2013-07-17

PDF

264

被引次数

15

摘要：

建立了高效液相色谱-串联质谱(HPLC-MS/MS)同时测定保健食品中23种违禁精神药品的检测方法。样品经甲醇超声振荡提取20 min,于12000 r/min下离心后进行HPLC-MS/MS分析检测。采用Agilent Eclipse Plus C18柱分离,流动相A为10 mmol/L甲酸铵溶液,流动相B为乙腈-甲醇(1:1, v/v)溶液,梯度洗脱;采用电喷雾离子源、正负离子模式切换、多反应监测(MRM)模式检测。23种精神药品在线性范围内线性关系良好,相关系数(R2)均大于0.990;检出限在0.02~1.0 μ g/L之间;3个添加水平的回收率为82.3%~114.8%,相对标准偏差(RSD)在1.3%~13.7%之间。样品筛查结果发现13种保健品中有1种样品非法添加了安宁,1种样品添加了奥沙西泮,2种样品添加了扎来普隆。该方法选择性强、灵敏度高、处理方法简单,可用于保健品中违禁镇静安神类化学药品的测定。

关键词: 保健食品, 高效液相色谱-串联质谱, 精神药品

Abstract:

An analytical method using HPLC-MS/MS was developed for qualitative and quantitative analysis of 23 sedative drugs in health foods. The method was based on the sonication-assisted extraction of the health food samples using 10 mL methanol. The extract was then isolated by centrifugation and the supernatant was separated on an Agilent Eclipse Plus C18 column with gradient elution at a flow rate of 300 μ L/min. A binary mobile phase was 10 mmol/L ammonium formate (solvent A) and acetonitrile/methanol (1:1, v/v; solvent B). The electrospray ionization (ESI) source in positive ion mode or negative ion mode was used for multiple reaction monitoring (MRM). The external standard method was used for the quantification. The calibration graphs were linear in their concentration ranges with the correlation coefficients more than 0.990. The limits of detection (LOD, S/N=3) were between 0.02-1.0 μ g/L. The recoveries for all the drugs in health foods were 82.3%-114.8% with the relative standard deviations less than 14.1% at three spiked levels. Thirteen kinds of health foods were tested, in which meprobamate and oxazepan were found in one sample separately, and zaleplon was found in two samples. The method is specific, sensitive, easy and quick and suitable for the confirmation and quantification of the 23 sedative drugs in health foods.

Key words: health foods, high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS), sedative drugs

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