食品科学

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超高效液相色谱-串联质谱法测定调节三高类保健食品中59种非法添加物

邵瑞婷1,丁学妍2,姜洁3   

  1. 1. 北京市食品安全监控和风险评估中心
    2. 北京市食品检验研究院(北京市食品安全监控和风险评估中心)
    3. 北京市食品安全监控中心
  • 收稿日期:2023-06-28 修回日期:2023-09-06 出版日期:2023-09-26 发布日期:2023-09-26
  • 通讯作者: 丁学妍

Determination of 59 illegal additives in three kinds of regulated health food by ultra high performance liquid chromatography-tandem mass spectrometry

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  • Received:2023-06-28 Revised:2023-09-06 Online:2023-09-26 Published:2023-09-26

摘要: 摘 要:建立了调节三高类保健食品中59种非法添加物的超高效液相色谱-串联质谱检测方法。样品经甲醇提取,QuEChERS净化,氮吹至近干,1mL 40%甲醇水(体积分数)复溶,UPLC-MS/MS测定,基质外标法定量。在ACQUITY UPLC HSS T3 反相柱上分离,梯度洗脱,流动相为乙腈和5mmol/L乙酸铵+0.1%甲酸水,质谱采集模式为多反应监测电喷雾正、负离子模式。结果表明:59非法添加物在线性范围内,相关系数(R)均大于0.99。该方法具有前处理方式较简单、分析时间较短、灵敏度好、准确度高、杂质干扰小等特点,可以用于调节三高类保健食品中多种非法添加物的检测。

关键词: 关键词:调节三高类保健食品, QuEChERS净化, 超高效液相色谱串联质谱, 非法添加

Abstract: Abstract: A super high performance liquid chromatography-tandem mass spectrometry detection method has been established to regulate the detection of 59 illegal additives in three high category health foods. The sample was extracted with methanol, purified with QuEChERS, blown to near dry with nitrogen, redissolved with 1mL of 40% methanol water (volume fraction), determined by UPLC-MS/MS, and quantified using matrix external standard method. It is separated on the ACQUITY UPLC HSS T3 reverse phase column and eluted in gradient. The mobile phase is acetonitrile and 5mmol/L Ammonium acetate+0.1% formic acid water. The mass spectrum acquisition mode is the multi reaction monitoring electrospray positive and negative ion mode. The results indicate that 59 illegal additives are within a linear range, and the correlation coefficients (R) are all greater than 0.99. This method has the characteristics of simple pre-treatment, short analysis time, good sensitivity, high accuracy, and low impurity interference, and can be used to regulate the detection of multiple illegal additives in three types of health food.

Key words: Keywords: Three kinds of regulated health food, QuEChERS purification, Added illegally, High-performance liquid chromatography tandem mass spectrometry

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