同位素稀释-固相萃取-LC/MS/MS法测定婴幼儿配方食品中双酚类化合物  

Determination of Bisphenol Substances Migration in Infant Food by Isotope Dilution-Solid Phase ExtractionLiquid Chromatography-tandem Mass Spectrometry

作　　者：高梦婕[1] 邓晓军[2] 曲栗[2] 曹晨[2] 周瑶[2] 赵善贞[2] 伊雄海[2] 韩丽[2] 丁卓平[1] 

机构地区：[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

出　　处：《分析化学》2015年第3期371-378,共8页Chinese Journal of Analytical Chemistry

基　　金：上海市科委技术标准专项项目(No.13DZ0502502);十二五重大仪器设备专项(No.2013YQ15055705);科技部"十二五"科技支撑项目(No.2012BAD33B02)资助

摘　　要：建立了同位素稀释-固相萃取-高效液相色谱-串联质谱法同时测定婴幼儿配方食品中14种双酚类化合物的方法。婴幼儿配方乳粉、婴幼儿配方谷粉和婴幼儿辅食果泥等试样经乙腈提取,Pro Elut PLS固相萃取小柱（500 mg/6 m L）净化,14种双酚类化合物经Waters Atlantis T3色谱柱（150 mm×2.1 mm,3.0μm）分离后,正负离子同时扫描模式下多反应监测（MRM）,基质匹配BPA-d16、TBBPA-d10和BPS-c13同位素内标法定量。结果表明,在线性范围内,14种双酚类化合物线性相关系数（r）均大于0.999,回收率为83.0%-107.1%（n=6）,相对标准偏差（RSD）为5.1%-9.8%（n=6）,方法的定量限（LOQ）为1.0-2.0μg/kg,检出限（LOD）为0.3-0.7μg/kg。方法操作简单、高效、重现性好,满足现行法规要求的同时,实现了婴幼儿食品中双酚类化合物的定性定量检测。A method based on isotope dilution-solid phase extraction（ SPE） and liquid chromatographytandem mass spectrometry（ HPLC-MS / MS） for the simultaneous determination of 14 bisphenol substances migration in infant food（ infant milk powder,infant nutritious cereal and infant supplement puree） was presented. The samples were extracted by acetonitrile followed by Pro Elut PLS（ 500 mg /6 m L） to remove matrix interference. The separations of 14 bisphenol substances were performed on a Waters Atlantis T3（ 150 mm × 2. 1 mm,3. 0 μm）,respectively,in the positive and negative MRM mode by HPLC-MS /MS.The quantification was carried out by matrix-matched calibration curve and internal standard（ BPA-d16,TBBPA-d10 and BPS-c13）. The results demonstrated that the calibration curves showed good linearity in each range and the correlation coefficients（ r） were greater than 0. 999. The average recoveries at three spiked levels were ranged from 83. 0% to 107. 1% with the relative standard deviations（ RSD） of 5. 1% to 9. 8%.The limits of quantitation（ LOQ,S / N10） were 1. 0-2. 0 μg / kg and the limits of detection（ LOD,S / N3）were in the range of 0. 3- 0. 7 μg / kg. The established method was simple,time-saving and efficient,and could meet the requirements for current regulations while achieving qualitative and quantitative determination of 14 bisphenol substances in infant food.

关 键 词：双酚类 婴幼儿食品 高效液相色谱-串联质谱法 同位素稀释 

分 类 号：TS207.3[轻工技术与工程—食品科学] O657.63[轻工技术与工程—食品科学与工程]