色谱

色谱 ›› 2017, Vol. 35 ›› Issue (12): 1257-1265.DOI: 10.3724/SP.J.1123.2017.09031

• 研究论文 • 上一篇    下一篇

QuEChERS-超高效液相色谱-串联质谱法同时测定保健食品中21种非法添加化学药物

郑佳1,3, 郗存显2, 曹淑瑞2, 王国民2, 唐柏彬2, 王智1,3, 母昭德1,3   

  1. 1. 重庆医科大学药学院, 重庆 400016;
    2. 重庆出入境检验检疫局重庆市进出口食品安全工程技术研究中心, 重庆 400020;
    3. 重庆市生物化学与分子药理学重点实验室, 重庆 400016
  • 收稿日期:2017-09-18 出版日期:2017-12-08 发布日期:2017-12-15
  • 通讯作者: 母昭德,E-mail:1281618155@qq.com
  • 基金资助:

    国家质量监督检验检疫总局科技计划项目（2016IK296）；重庆市科学技术委员会青-科学基金专项项目（cstc2014kjrc-qnrc00002）.

Determination of 21 illegally added chemical drugs in health foods using ultra performance liquid chromatography-tandem mass spectrometry coupled with QuEChERS

ZHENG Jia1,3, XI Cunxian2, CAO Shurui2, WANG Guomin2, TANG Bobin2, WANG Zhi1,3, MU Zhaode1,3   

  1. 1. College of Pharmacy, Chongqing Medical University, Chongqing 400016, China;
    2. Chongqing Entry-Exit Inspection and Quarantine Bureau Chongqing Engineering Technology Research Center of Import and Export Food Safety, Chongqing 400020, China;
    3. Chongqing Key Laboratory of Biochemistry and Molecular Pharmacology, Chongqing 400016, China
  • Received:2017-09-18 Online:2017-12-08 Published:2017-12-15
  • Supported by:

    Science and Technology Project of General Administration of Quality Supervision, Inspection and Quarantine of the People's Republic of China (No. 2016IK296); Youth Science and Technology Talents Fund Project of Chongqing Municipal Science and Technology Commission (No. cstc2014kjrc-qnrc00002).

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164

被引次数

4

摘要：

建立了QuEChERS-超高效液相色谱-串联质谱测定改善睡眠类和提高免疫力类保健食品中21种非法添加化学药物的分析方法。口服液、保健酒分别用乙腈和乙腈-水-甲酸（60：39：1，v/v/v）振荡提取，QuEChERS法净化；采用Acquity UPLCTM BEH C18色谱柱（50 mm×2.1 mm，1.7 μm）分离，以乙腈和2 mmol/L乙酸铵溶液（含0.1%（v/v）甲酸）为流动相进行梯度洗脱；在电喷雾离子源正离子模式（ESI+）下电离，多反应监测（MRM）模式检测。结果表明，21种化学药物在1~100 μg/L范围内线性关系良好，相关系数（R2）均≥ 0.992，检出限（LOD）为0.07~3.41 μg/kg，定量限（LOQ）为0.22~11.36 μg/kg。3种加标水平（10、20和100 μg/kg）下，21种化学药物在口服液和保健酒中的平均加标回收率分别为61.4%~116.5%和67.4%~98.4%；相对标准偏差（RSD）分别为0.2%~13.4%和0.2%~11.8%。该法简便，灵敏性高，实用性强，可用于改善睡眠和提高免疫力类保健食品中21种非法添加化学药物的检测。

关键词: QuEChERS, 保健食品, 超高效液相色谱-串联质谱, 化学药物

Abstract:

A method for the simultaneous determination of 21 illegally added chemical drugs in improving sleep and immunity health foods using ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) was developed. Oral liquid and health wine samples were shaken with acetonitrile and acetonitrile-water-formic acid (60:39:1, v/v/v), respectively, then purified by QuEChERS method. The extracts were separated on an Acquity UPLCTM BEH C18 column (50 mm×2.1 mm, 1.7 μm) with gradient elution of acetonitrile and 2 mmol/L ammonium acetate solution containing 0.1% (v/v) formic acid as mobile phases. The electrospray ionization in positive ion mode was used for analysis in multiple reaction monitoring (MRM) mode. The results showed that the target drugs had a good linear relationship in the range of 1-100 μg/L with the correlation coefficients (R2) ≥ 0.992. The limits of detection (LODs) and limits of quantification (LOQs) were 0.07-3.41 μg/kg and 0.22-11.36 μg/kg, respectively. The average recoveries of the 21 chemical drugs in oral liquid and health wine were in the range of 61.4%-116.5% and 67.4%-98.4% with the relative standard deviations (RSDs) of 0.2%-13.4% and 0.2%-11.8%, respectively. The developed method is sensitive and reliable. It has been successfully used for the detection of illegally added chemical drugs in real samples.

Key words: chemical drugs, health foods, QuEChERS, ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS)

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