色谱

色谱 ›› 2019, Vol. 37 ›› Issue (7): 701-711.DOI: 10.3724/SP.J.1123.2019.01046

• 研究论文 • 上一篇    下一篇

QuEChERS法结合液相色谱-串联质谱测定保健食品中50种非食用添加物

胡胜杰1, 李优2, 周莹3, 伊雄海2, 邓晓军2, 陈沁1, 徐敦明4, 钮冰1   

  1. 1. 上海大学生命科学学院食品工程系, 上海 200444;
    2. 上海出入境检验检疫局动植物与食品检验检疫技术中心, 上海 200135;
    3. 上海杉达学院, 上海 201209;
    4. 厦门出入境检验检疫局检验检疫技术中心, 福建 厦门 361012
  • 收稿日期:2019-01-26 出版日期:2019-07-08 发布日期:2015-05-21
  • 通讯作者: 李优.Tel:(021)38620524,E-mail:liyou@shciq.gov.cn.
  • 基金资助:
    国家重点研发计划项目（2017YFF0211003，2018YFC1603603）；中央引导地方专项（YDZX20173100004528）；福建社会发展引导性重点项目（2017Y0077）；厦门市科技项目（3502Z20174040）.

Determination of 50 non-edible additives in health food using the QuEChERS method and liquid chromatography-tandem mass spectrometry

HU Shengjie1, LI You2, ZHOU Ying3, YI Xionghai2, DENG Xiaojun2, CHEN Qin1, XU Dunming4, NIU Bing1   

  1. 1. Department of Food Engineering, School of Life Science, Shanghai University, Shanghai 200444, China;
    2. Animal, Plant and Food Inspection & Quarantine Center, Shanghai Entry-Exit Inspection and Quarantine Bureau, Shanghai 200135, China;
    3. Sanda University, Shanghai 201209, China;
    4. Inspection and Quarantine Technology Center, Xiamen Entry-Exit Inspection and Quarantine Bureau, Xiamen 361012, China
  • Received:2019-01-26 Online:2019-07-08 Published:2015-05-21
  • Supported by:
    National Key Research and Development Plan Project (Nos. 2017YFF0211003, 2018YFC1603603); Central Guiding Local Special Projects (No. YDZX20173100004528); Social Development Guiding Priority Project of Fujian Province (No. 2017Y0077); Science and Technology Project of Xiamen (No. 3502Z20174040).

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摘要： 建立了液相色谱-串联质谱法测定保健食品中50种非食用添加物的分析方法。样品经甲醇提取，QuEChERS法净化，Agilent Phoroshell SB C18柱（150 mm×3.0 mm，2.7 μm）分离，并以0.1%（v/v）甲酸水溶液与乙腈为流动相，梯度洗脱，电喷雾正离子模式和负离子模式同时扫描，多反应监测模式（MRM）检测。结果表明，50种化合物均得到较好的分离，线性范围内基质匹配标准溶液的线性关系良好（r2>0.99）。方法的检出限（LOD，S/N≥3）与定量限（LOQ，S/N≥10）分别为0.010~1 mg/kg和0.02~2 mg/kg。考察了50种非食用添加物在5种典型保健食品基质（口服液、片剂、膏剂、丸剂、胶囊）中的加标回收率，在1 LOQ、2 LOQ、10 LOQ加标水平的平均回收率为63.1%~115.7%，相对标准偏差（RSD）均不大于8.9%（n=6）。该方法简单、灵敏度高且实用性强，适用于保健食品中50种非食用添加物的确证。

关键词: QuEChERS, 保健食品, 非食用添加物, 液相色谱-串联质谱

Abstract: A liquid chromatography-tandem mass spectrometry (LC-MS/MS) method was established for the determination of 50 non-food additives in health food. The samples were extracted with methanol and purified using the QuEChERS method. The separation was performed on an Agilent Phoroshell SB C18 column (150 mm×3.0 mm, 2.7 μm) with a mobile phase of 0.1% (v/v) formic acid aqueous solution and acetonitrile. The determination was performed by MS/MS in positive or negative electrospray ionization and multiple reaction monitoring mode. The results demonstrated that all 50 compounds could be well separated with a good linear relationship (r2>0.99). The limits of detection (LODs, S/N ≥ 3) and limits of quantification (LOQs, S/N ≥ 10) were in the range of 0.010-1 mg/kg and 0.020-2 mg/kg, respectively. The matrix effects in five kinds of typical health foods (oral liquid, tablets, ointments, pills, and capsules) were evaluated and reduced by means of matrix matching. At the spiked levels of 1 LOQ, 2 LOQ, and 10 LOQ, the recoveries of all drugs varied from 63.1% to 115.7% with relative standard deviations (RSDs) of no more than 8.9% (n=6). The method is simple, sensitive, practical, and suitable for monitoring 50 non-edible additives in health food.

Key words: health food, liquid chromatography-tandem mass spectrometry (LC-MS/MS), non-edible additives, QuEChERS

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