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乳业科学与技术 ›› 2017, Vol. 40 ›› Issue (4): 15-19.DOI: 10.15922/j.cnki.jdst.2017.04.004

• 分析检测 • 上一篇    下一篇

稳定同位素内标-高效液相色谱-串联质谱法测定婴幼儿食品中双酚类化合物

耿宁, 卢剑   

  1. 江苏省质量协会, 江苏 南京 210029; 江苏省产品质量监督检验研究院, 江苏 南京 210007, 江苏省产品质量监督检验研究院, 江苏 南京, 210007
  • 出版日期:2017-07-01 发布日期:2021-12-15

Evaluation of Bisphenols Residues in Infant Foods by High Performance Liquid Chromatography-Tandem Mass Spectrometry Using Stable Isotope Internal Standard

GENG Ning, LU Jian   

  1. (1.Quality Association of Jiangsu Province, Nanjing 210029, China; 2.Jiangsu Product Quality Inspection and Testing Institute, Nanjing 210007, China)
  • Online:2017-07-01 Published:2021-12-15

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摘要： 为建立同时测定婴幼儿配方食品中4种双酚类化合物(双酚A(bisphenol A,BPA)、双酚B(bisphenol B,BPB)、双酚F(bisphenol F,BPF)和双酚S(bisphenol S,BPS))的高效液相色谱-串联质谱(high performance liquid chromatography-tamdem mass spectrometry,HPLC-MS/MS)分析方法,分别对提取溶剂、色谱柱类型、MS参数和流动相进行优化,在优化后的最优实验条件下,对样品进行HPLC-MS/MS检测,同时进行方法学评价。结果表明:4种双酚类化合物在质量浓度为5.0～200.0μg/L范围内的线性关系良好,R2均大于0.9970,方法检出限(limit of detection,LOD)为1.5μg/kg;阴性样品中4种目标化合物的加标回收率(3个添加水平中各化合物的质量浓度分别为5.0、10.0、50.0μg/L)在84.0％～106.5％之间,相对标准偏差(relative standard deviation,RSD)为1.6％～6.4％。该方法净化效果好、灵敏度高、精密度良好、定量准确,适用于婴幼儿食品中双酚类化合物的定性及定量检测。

关键词: 高效液相色谱-串联质谱法; 双酚类化合物; 婴幼儿食品; 环境激素

Abstract: An isotope internal standard coupled with high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) method was established for the simultaneous determination of four bisphenols (bisphenols A, B, F and S) in infant foods. Samples were extracted with a mixture of ethyl acetate and cyclohexane and detected by HPLC-MS/MS in the multi-reaction monitoring mode. Under the optimized conditions, the four bisphenols showed good linearity in the range of 5.0–200.0 μg/L with R2 larger than 0.9970. The detection limit of the method was 1.5 μg/kg. The mean recoveries of negative samples spiked at three concentration levels (5.0, 10.0 and 50.0 μg/L) were in the range of 84.0％–106.5％with relative standard deviations (RSDs, n = 6) ranging from 1.6％ to 6.4％. The proposed method had the advantages of high sensitivity, good purification efficiency and quantitative accuracy and it was suitable for the detection of bisphenols in infant foods.

Key words: high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS); bisphenols; infant foods; environmental hormones

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