液相色谱-串联质谱法测定液体乳制品中7种激素残留  

Determination of Seven Residual Hormones in Fluid Dairy Products by Liquid Chromatography-Tandem Mass Spectrometry

作　　者：万春花[1] 张云伟[1] 黄优生[1] 鄢兵[1] 胡海山[1] 刘延华[1] 熊文生[1] 

机构地区：[1]江西省分析测试研究所,江西南昌330029

出　　处：《现代科学仪器》2016年第5期83-87,共5页Modern Scientific Instruments

基　　金：江西省科技支撑计划-社会发展,项目编号：20111BBG70010-2

摘　　要：建立了液相色谱-串联四极杆质谱同时测定液体乳制品中雌二醇、雌三醇、雌酮、已烯雌酚、双烯雌酚、己烷雌酚和孕酮7种激素残留的快速测定方法。采用甲醇提取液体乳制品中待测定组分，提取液经离心、C18固相萃取柱净化、甲醇洗脱。在正、负电喷雾离子化多反应监测模式下检测7种激素，采用ZORBAX SB—C18（2．1×μ1OOmm，3．5μm）色谱柱，流动相为乙腈-5mmol／L乙酸铵溶液、乙腈-0．1％甲酸溶液，外标法定量。在该优化条件下，7种激素定量限（S／N≥10）为1μg／kg～20μg／kg，方法回收率为77．2％～89．6％，相对标准偏差（厅印）为5．61％～8．49％。经测定多种市场上销售的液体乳制品，表明该方法操作简单、测定结果准确，可以用于液体乳制品中多种激素残留的快速测定。A methodology has been developed to rapidly quantify the residues of seven hormones in fluid dairy products by liquid chromatography-tandem quadrupole mass spectrometry （LC-MS/MS）, including estradiol, estrio!, estrone, diethylstilbestrol, dienestrol, hexestrol and progesterone, etc. The lipids in the samples were extracted using methanol, centrifuged and purified on a C18 solid-phase extraction columns with methanol as the elution solvent. The analysis of the seven analytes was carried out using LC-MS/MS on a ZORBAX SB-C18 column with the MS detector in positive and negative electrospray multi-reaction monitoring mode. For negative ESI mode, Acetonitrile-5mmol/L ammonium acetate solution was used as mobile phase while Acetonitrile-0.1% formic acid solution was used as mobile in the positive ESI mode. The quantification was based on external standards. At these optimal conditions, the limits of quantification （S/N≥10） were 1 μg/kg - 20 μg/kg. The overall recoveries varied from 77.2% to 89.6%, and the relative standard deviations were between 3.61% and 8.49%. Tests on commercial fluid dairy products demonstrated the simplicity and accuracy of this methodology, which can be used for determining the residual hormones in fluid dairy products.

关 键 词：液相色谱-串联质谱 固相萃取 激素 液体乳制品 

分 类 号：O657.63[理学—分析化学]