超高效液相色谱-串联质谱法测定动物肌肉组织中的14种激素  

Determination of fourteen hormones in animal muscle tissues using ultra-perform liquid chromatography tandem mass spectrometry

作　　者：陈君慧[1] 路勇[2] 冯楠[2] 姜洁[2] 谢文东[2] 江英[1] 赵俊平[2] 鲁绯 

机构地区：[1]石河子大学食品学院,新疆石河子832000 [2]北京市食品安全监控中心,北京100041 [3]北京市食品及酿酒产品质量监督检验一站,北京100075

出　　处：《食品工业科技》2013年第8期74-79,共6页Science and Technology of Food Industry

基　　金：北京市科委课题(Z1111000774211019)

摘　　要：建立了超高效液相色谱-串联质谱（UPLC—MS／MS）同时测定动物肌肉组织中的14种激素残留量的分析方法。试样经乙酸乙酯提取，固相萃取法净化后，以甲醇和乙酸铵甲酸缓冲溶液为流动相，进行梯度洗脱，HSST3液相色谱柱分离，采用多反应监测（MRM）模式，外标法定量，正负离子同时扫描检测。结果表明，14种激素的方法检出限为0_3～1．0μg／kg；在0．5～50μg／kg线性范围内，线性关系良好，相关系数均大于0．99；添加2、5、10μg／kg3个不同浓度水平的平均回收率在72．48％～114．52％之间，相对标准偏差（RSD）在3．93％～11．17％之间。该方法具有灵敏度高，结果准确，选择性好等特点，可以满足动物肌肉组织中多种激素残留的同时泖1定。A credible method was developed for the simultaneous determination of fourteen hormones residues in animal muscle tissues based on ultra-performance liquid chromatography tandem mass spectrometry （UPLC-MS/MS）. Samples were extracted with ethyl acetate,followed by clean up based on solid phase extraction（SPE）. After HSS T3 gradient elution separation using methanol and formic solution as mobile phase. Eluents were qualitatively and quantitatively determined under multiple reaction monitoring （MRM） scan type with Ultra-perform liquid chromatography tandem mass spectrometry with switching ESI＋/ESI-. The result showed that the limits of detection（LOD） of 14 hormones were 0.3-1.0μg/kg. Recoveries at 0.5-50μg/kg levels and the relative standard deviations （RSD） were 72.48%- 114.52% and 3.93% -11.17%, respectively. This method was sensitive,accurate and specific,and was appropriate for the identification and quantification of hormones in animal muscle tissues.

关 键 词：超高效液相色谱-串联质谱 激素 残留分析 

分 类 号：TS207.3[轻工技术与工程—食品科学]