色谱

色谱 ›› 2019, Vol. 37 ›› Issue (7): 778-785.DOI: 10.3724/SP.J.1123.2019.01016

• 技术与应用 • 上一篇    

固相萃取-超高效液相色谱-串联质谱法同时测定保健食品中21种非法添加化合物

徐敦明1, 赖国银1, 陈燕1, 罗超1, 伊雄海2, 邓晓军2, 冯峰3, 张峰3   

  1. 1. 厦门海关技术中心, 福建 厦门 361026;
    2. 上海海关动植物与食品检验检疫技术中心, 上海 200135;
    3. 中国检验检疫科学研究院食品安全研究所, 北京 100123
  • 收稿日期:2019-01-21 出版日期:2019-07-08 发布日期:2015-05-21
  • 通讯作者: 赖国银.Tel:(0592)6803438,E-mail:gylai_ustc@163.com.
  • 基金资助:
    国家重点研发计划（2017YFC1601606，2017YFF0211003）；福建社会发展引导性（重点）项目（2017Y0077）；厦门市科技项目（3502Z20174040）.

Simultaneous determination of 21 illegally added compounds in health foods by ultra high performance liquid chromatography-tandem mass spectrometry with solid phase extraction

XU Dunming1, LAI Guoyin1, CHEN Yan1, LUO Chao1, YI Xionghai2, DENG Xiaojun2, FENG Feng3, ZHANG Feng3   

  1. 1. Technical Center of Xiamen Customs, Xiamen 361026, China;
    2. Technical Center for Animal Plant and Food Inspection and Quarantine, Shanghai Customs, Shanghai 200135, China;
    3. Institute of Food Safety, Chinese Academy of Inspection and Quarantine, Beijing 100123, China
  • Received:2019-01-21 Online:2019-07-08 Published:2015-05-21
  • Supported by:
    National Key Research and Development Program of China (Nos. 2017YFC1601606, 2017YFF0211003); Guiding (Key) Project of Social Development of Fujian (No. 2017Y0077); Science and Technology Project of Xiamen (No. 3502Z20174040).

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摘要： 建立了固相萃取-超高效液相色谱-串联质谱同时测定保健食品中21种非法添加化合物的方法。样品用乙腈超声提取后，采用HLB固相萃取小柱净化，经Waters BEH C18色谱柱（100 mm×2.1 mm，1.7 μm）分离，以10 mmol/L乙酸铵和甲醇为流动相进行梯度洗脱，采用电喷雾电离（ESI）源，在多反应监测模式下检测。结果表明，21种非法添加化合物均呈良好的线性关系，相关系数均≥0.995，不同基质的检出限为3~160 μg/kg，回收率为61.8%~109.3%，相对标准偏差为1.6%~14.7%。该方法可用于减肥类、降脂类、降糖类、降压类保健食品中21种非法添加药物的同时测定。

关键词: 保健食品, 超高效液相色谱-串联质谱, 非法添加, 固相萃取

Abstract: A rapid method for the simultaneous determination of 21 illegally added compounds in health foods was developed based on solid phase extraction (SPE) combined with ultra high performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS). After ultrasonic extraction with acetonitrile, the samples were purified on an HLB SPE column, separated on a Waters BEH C18 column (100 mm×2.1 mm, 1.7 μm) using 10 mmol/L ammonium acetate aqueous solution and methanol as the mobile phases. The compounds were detected by an electrospray ionization (ESI) source in positive ion mode with multi-reaction monitoring (MRM). The 21 illegal additives showed good linear relationships with correlation coefficients no less than 0.995. The limits of detection (LODs) were 3-160 μg/kg for different matrixes. The recoveries ranged from 61.8% to 109.3%, and the relative standard deviations ranged from 1.6% to 14.7%. The method can be used for the simultaneous determination of the illegally added drugs in the losing weight, lipid-lowering, anti-diabetic and anti-hypertension health foods.

Key words: health foods, illegally additives, solid phase extraction (SPE), ultra high performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS)

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