食品科学 ›› 2024, Vol. 45 ›› Issue (9): 232-242.doi: 10.7506/spkx1002-6630-20230628-221

• 安全检测 • 上一篇    下一篇

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种非法添加药物

邵瑞婷,丁学妍,姜洁   

  1. (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),国家市场监管重点实验室(食品安全重大综合保障关键技术),北京 100041)
  • 出版日期:2024-05-15 发布日期:2024-05-01

Determination of 59 Illegally Added Drugs in Health Foods with Hypoglycemic, Hypolipidemic and Antihypertensive Activity by Ultra-high Performance Liquid Chromatography-Tandem Mass Spectrometry

SHAO Ruiting, DING Xueyan, JIANG Jie   

  1. (Key Laboratory of Key Technologies of Major Comprehensive Guarantee of Food Safety for State Market Regulation, Beijing Institute of Food Inspection and Research (Beijing Municipal Center for Food Safety Monitoring and Risk Assessment), Beijing 100041, China)
  • Online:2024-05-15 Published:2024-05-01

摘要: 本实验建立了调节三高类保健食品中59 种非法添加药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,1 mL 40%甲醇溶液(体积分数)复溶,以乙腈和0.1%甲酸溶液(5 mmol/L乙酸铵)为流动相,经ACQUITY UPLC HSS T3反相柱梯度分离,超高效液相色谱-串联质谱在正、负离子模式下多反应监测,采用基质外标法定量。结果表明:59 种非法添加药物在线性范围内,决定系数(R2)均大于0.980,回收率在60.2%~119.5%之间,相对标准偏差在1.2%~15.0%之间。该方法具有前处理较简单、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药物的检测。

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;非法添加药物

Abstract: An analytical method using ultra-high performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) was established for the detection of 59 illegally added drugs in health foods with hypoglycemic, hypolipidemic and antihypertensive activity. Samples were extracted with methanol, and the extract was purified by the quick, easy, cheap, effective, rugged, and safe (QuEChERS) method and blown to dryness under nitrogen gas. The residue was dissolved in 1 mL of 40% (V/V) methanol aqueous solution. The chromatographic separation was performed using reverse-phase chromatography on an ACQUITY UPLC HSS T3 column through gradient elution using a mobile phase consisting of acetonitrile and 0.1% aqueous formic acid (containing 5 mmol/L ammonium acetate). The mass spectrometer was operated in both the positive and negative ion modes using multi-reaction monitoring (MRM), and quantitative analysis was performed using a matrix-matched external standard method. The results showed that the calibration curves for the 59 illegally added drugs were linear with coefficient of determination (R2) greater than 0.980. Recoveries ranged from 60.2% to 119.5%, and relative standard deviations (RSDs) ranged from 1.2% to 15.0%. This method is characterized by simple pre-treatment, short analysis time, good sensitivity, high accuracy, and low impurity interference, and can be used to the detection of multiple illegal drugs in health foods with hypoglycemic, hypolipidemic and antihypertensive activity.

Key words: health foods with hypoglycemic, hypolipidemic and antihypertensive activity; quick, easy, cheap, effective, rugged, and safe purification; ultra-high performance liquid chromatography-tandem mass spectrometry; illegal addition of drugs

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