液质联用法测定婴儿乳粉中双酚A和己烯雌酚  

Determination of Bisphenol A and Diethylstilbestrol in Infant Milk Powder by LC-MS/MS

作　　者：刘艳琴[1] 王浩[1] 杨红梅[1] 郭启雷[1] 史海良[1] 田艳玲[1] 

机构地区：[1]国家食品质量安全监督检验中心,北京100094

出　　处：《食品研究与开发》2013年第17期80-83,共4页Food Research and Development

基　　金：国家质检总局质检公益性行业科研专项资助项目(200910267-02)资助项目

摘　　要：建立了婴儿乳粉中双酚A和己烯雌酚残留的高效液相色谱-串联四极杆质谱联用测定方法。样品经碱性乙腈超声提取,以MGⅢ-C18色谱柱(2.1×150 mm,1.8μm)分离,流动相为10 mmol/L乙酸铵水溶液和甲醇(梯度洗脱),流速0.25 mL/min。采用多反应监测负离子模式,可以同时对婴幼儿配方乳粉中的双酚A和己烯雌酚进行定性和定量测定。方法在1.0μg/L^25.0μg/L范围内呈良好线性,方法的检出限为5μg/kg。在5、25、250μg/kg三个加标水平下,加标回收率为80.6%~102.9%,相对标准偏差为1.29%~8.83%。A quick confirrnative method was developed for determining the residues of Bisphenol A and diethylstilbestrol in infant milk powder by LC-MS/MS. The sample was ultrasonic extracted with alkaline acetonitrile, the HPLC separation was carried out on a MG Ⅲ-C18 column （2.1 ~ 150 mm, 1.8 Ixm） , the mobile phase were 10 mmol/L ammonium acetate solution and methanol with gradient elution, the flow was 0.25 mL/min. The detection of Bisphenol A and diethylstilbestrol was carried outin the negative multi-reaction monitoring （MRM）mode. Under the optimal conditions, good linear relationship was obtained in the range of 1.0 μg/L- 25.0 Ixg/L for Bisphenol A and diethylstilbestrol.The limit of detection was 5 μg/kg. The recoveries at three spiked levels of 5,25,250 μg/kg were between 80.6 % and 102.9 %, and RSDs value were between 1.29 % and 8.83 %.

关 键 词：液质联用仪 婴儿配方乳粉 双酚A 己烯雌酚 

分 类 号：TS252.7[轻工技术与工程—农产品加工及贮藏工程] O657.63[轻工技术与工程—食品科学与工程]