色谱

色谱 ›› 2018, Vol. 36 ›› Issue (12): 1245-1260.DOI: 10.3724/SP.J.1123.2018.06025

• 研究论文 • 上一篇    下一篇

超高效液相色谱-串联质谱法测定茶叶、代用茶和饮料食品中63种非法添加化合物

唐维英1,2, 黄泽玮1, 钱广生2, 魏宇涛1, 黄瑛1, 徐小平2, 余晓琴1   

  1. 1. 四川省食品药品检验检测院, 四川 成都 610097;
    2. 四川大学华西药学院, 四川 成都 610041
  • 收稿日期:2018-07-02 出版日期:2018-12-08 发布日期:2014-11-06
  • 通讯作者: 余晓琴,Tel:(028)87877142,E-mail:113343838@qq.com
  • 基金资助:

    “食品安全关键技术研发”重点专项（2017YFC1601300）；国家食品药品监督管理总局研究项目.

Determination of 63 compounds illegally added in tea, substitute tea and beverage foods by ultra-high performance liquid chromatography-tandem mass spectrometry

TANG Weiying1,2, HUANG Zewei1, QIAN Guangsheng2, WEI Yutao1, HUANG Ying1, XU Xiaoping2, YU Xiaoqin1   

  1. 1. Sichuan Provincial Institute for Food and Drug Control, Chengdu 610097, China;
    2. West China School of Pharmacy, Sichuan University, Chengdu 610041, China
  • Received:2018-07-02 Online:2018-12-08 Published:2014-11-06
  • Supported by:

    National Special Project for "Key Science and Technology for Food Safety" (No. 2017YFC1601300); Research Project of China Food and Drug Administration.

PDF

81

摘要：

建立了超高效液相色谱-串联质谱（UPLC-MS/MS）同时测定茶叶、代用茶和饮料食品中63种非法添加化合物的分析方法。样品经甲醇超声提取后，采用Thermo Acclaim RSLC C18色谱柱（100 mm×2.1 mm，2.2 μm）分离，以5 mmol/L甲酸铵溶液（含体积分数为0.1%的甲酸）-0.1%（体积分数）甲酸乙腈为流动相进行梯度洗脱。在电喷雾离子源正离子模式下，采用动态多反应监测（dMRM）方式测定，外标法定量。63种待测化合物在相应的线性范围内呈良好的线性关系，相关系数（R2）均大于0.99；定量限为0.10~2.50mg/kg；在3个添加水平下，63种待测物的平均回收率为62.4%~129.4%，进样精密度和重复性的相对标准偏差为0.3%~9.6%（n=6）。该方法简便快捷、准确可靠，适用于茶叶、代用茶和饮料食品中非法添加具有解热镇痛效果的化合物检测。

关键词: 超高效液相色谱-串联质谱, 非法添加, 解热镇痛, 食品

Abstract:

A method based on ultra-high-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) was developed for the simultaneous determination of 63 compounds illegally added in tea, substitute tea, and beverage products. The samples were extracted by ultrasonic extraction using methanol, and the analytes were separated on the Thermo Acclaim RSLC C18 chromatographic column (100 mm×2.1 mm, 2.2 μm) by gradient elution using 5 mmol/L ammonium formate solution containing 0.1% (v/v) formic acid and 0.1% (v/v) formic acid acetonitrile as the mobile phase. The electrospray ion source was operated in the positive ion mode using the dynamic multi-reaction monitoring (dMRM) method, and the results were quantified by the external standard method. The correlation coefficients (R2) of the linear calibration curves were greater than 0.99 in the corresponding mass concentration ranges, and the limits of quantification (LOQs) for the analytes were 0.10-2.50 mg/kg. The average recoveries at three spiked levels ranged from 62.4% to 129.4%. The RSDs of the injection precision and the repeatability of samples were in the range 0.3%-9.6% (n=6). Thus, the proposed method is simple, rapid, accurate, reliable, and applicable for the detection of the illegal addition of antipyretic and analgesic affect compounds in tea, substitute tea and beverage food.

Key words: antipyretic and analgesic, food, illegal addition, ultra-high performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS)

中图分类号: