色谱

色谱 ›› 2014, Vol. 32 ›› Issue (11): 1201-1208.DOI: 10.3724/SP.J.1123.2014.06037

• 研究论文 • 上一篇    下一篇

QuEChERS法结合高效液相色谱-串联质谱法测定保健食品中12种双酚类化合物

高梦婕1, 周瑶2, 盛永刚2, 赵善贞2, 邓晓军2, 郭德华2, 丁卓平1, 王国民3, 彭涛4   

  1. 1. 上海海洋大学食品学院, 上海 201306;
    2. 上海出入境检验检疫局, 上海 200135;
    3. 重庆出入境检验检疫局, 重庆 400020;
    4. 中国检验检疫科学研究院, 北京 100123
  • 收稿日期:2014-06-25 修回日期:2014-08-19 出版日期:2014-11-08 发布日期:2014-10-31
  • 通讯作者: 丁卓平,E-mail:zpding@shou.edu.cn;邓晓军,Tel:(021)38620522,E-mail:E-mail:dengxj@shciq.gov.cn.
  • 基金资助:

    上海市科委技术标准专项项目(13DZ0502502,12DZ0503102);科技部"十二五"科技支撑项目(2012BAD33B02);国家质检总局质检公益专项(201310140-02).

Determination of 12 bisphenol substances in functional foods by QuEChERS and high performance liquid chromatography-tandem mass spectrometry

GAO Mengjie1, ZHOU Yao2, SHENG Yonggang2, ZHAO Shanzhen2, DENG Xiaojun2, GUO Dehua2, DING Zhuoping1, WANG Guomin3, PENG Tao4   

  1. 1. College of Food Science and Technology, Shanghai Ocean University, Shanghai 201306, China;
    2. Shanghai Entry-Exit Inspection and Quarantine Bureau, Shanghai 200135, China;
    3. Chongqing Entry-Exit Inspection and Quarantine Bureau, Chongqing 400020, China;
    4. Chinese Academy of Inspection and Quarantine, Beijing 100123, China
  • Received:2014-06-25 Revised:2014-08-19 Online:2014-11-08 Published:2014-10-31

PDF

176

被引次数

1

摘要：

建立了采用高效液相色谱-串联质谱(HPLC-MS/MS)同时测定粉剂、片剂和胶囊剂等保健食品中12种双酚类化合物的检测方法。样品中双酚类化合物经1%(v/v)乙酸乙腈溶液提取,QuEChERS方法净化;12种化合物经Thermo Aquasil C18色谱柱(150 mm×4.6 mm,3.0 μm)分离后,分别在串联质谱正、负离子多反应监测(MRM)模式下检测,基质匹配外标法定量。研究结果表明,在0.5~50.0 μg/kg内,12种双酚类化合物的线性相关系数均大于0.99,方法的检出限(S/N>3)为0.1~0.5 μg/kg,定量限(S/N>10)为0.4~1.7 μg/kg,不同基质的保健食品在3个添加水平(2.0、5.0和10.0 μg/kg)下的回收率为60.5%~116.3%(n=6),相对标准偏差(RSD)为6.8%~11.2%(n=6)。方法操作简单、耗时短、灵敏度高,满足现行法规要求,可实现保健食品中双酚类化合物的定性和定量测定。

关键词: QuEChERS, 保健食品, 高效液相色谱-串联质谱法, 双酚类化合物

Abstract:

A method based on high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) for the simultaneous determination of 12 bisphenol substances in functional foods (powder, tablet, capsule) was presented. The samples were extracted by acetonitrile containing 1% (v/v) acetic acid followed by further cleaned up using matrix solid-phase dispersion to remove matrix interferences. The separation of the 12 bisphenol substances was performed on a Thermo Aquasil C18 column (150 mm×4.6 mm, 3.0 μm), and determined in the positive and negative MRM modes by MS/MS using matrix-matched external standard method. The results demonstrated that the calibration curves were of good linearity with the correlation coefficients greater than 0.99. The limits of detection (LODs, S/N>3) were in the range of 0.1-0.5 μg/kg and the limits of quantitation (LOQs, S/N>10) were 0.4-1.7 μg/kg. The recoveries of the 12 bisphenol substances spiked at three levels (2.0, 5.0 and 10.0 μg/kg) in matrix ranged from 60.5% to 116.3% with the relative standard deviations (RSDs) of 6.8% to 11.2%. The established method is simple, time-saving and sensitive. It can meet the requirements for current regulations while achieving qualitative and quantitative determination of the 12 bisphenol substances in functional foods.

Key words: bisphenol substances, functional food, high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS), QuEChERS

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