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

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

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0.997 0,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。

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 0.997 0. 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.