QuEChERS净化-高效液相色谱-串联质谱法测定蜂蜜中农药及抗生素的含量  

Determination of Pesticides and Antibiotics in Honey by QuEChERS-HPLC-MS/MS

作　　者：苗琼晨 聂晶[1] 吴慧珍[1] 钱鸣蓉[2] 孙彩霞[2] 李祖光[1] 

机构地区：[1]浙江工业大学化学工程学院,杭州310014 [2]浙江省农业科学院质量标准研究所,杭州310021

出　　处：《理化检验（化学分册）》2017年第7期745-752,共8页Physical Testing and Chemical Analysis(Part B:Chemical Analysis)

基　　金：浙江省自然科学基金项目(LY16B050008);浙江省科技厅公益项目(2015C32006);农业部农药残留检测重点实验室资助项目(2014PRG01);杭州市钱江特聘专家项目(2014)

摘　　要：样品经pH 4.0的Na_2EDTA-Mcllvaine缓冲溶液稀释后,用乙酸-乙腈(1+19)混合溶液提取样品中农药及抗生素后,提取液中加入盐析剂分层,上清液放入盛有磁性C_(18)和N-丙基乙二胺吸附剂的净化瓶中净化,采用Luna C_(18)色谱柱,以不同体积比的0.1%(体积分数)甲酸溶液和乙腈组成的混合液为流动相进行梯度洗脱。以电喷雾正离子源和多反应监测模式进行质谱分析。30种化合物的质量分数在一定范围内与峰面积呈线性关系,检出限(3S/N)在0.3~4.1μg·kg^(-1)之间。按标准加入法进行回收试验,回收率在71.1%~116%之间,测定值的相对标准偏差(n=5)在0.80%~21%之间。The sample was diluted with pH 4. 0 of Na2EDTA-Mcllvaine buffer solution, and pesticides and antibiotics in the sample were extracted with a mixture of acetic aeid-acetonitrile （12-19）, and the extrael was stratified by salting-out agents. The supernatant was cleaned up with purification pipe filled with magnetic C18 and PSA. Luna C18 column was used as stationary phase, and a mixture of 0. 1% （φ） formic acid solution and acetonitrile in various ratios as mobile phase in gradient elution. ESI＋ and MRM were adopted in MS. I.inear relationships between values of peak area and mass concentration of 30 compounds were found in definite ranges, with detection limits （3S/N） in the range of 0. 3--4. 1μg · kg ^-1. Test for recovery was made by standard addition method, giving results in the range of 71.1^--116~, with RSDs （n=5） ranged from 0.80% to 21%.

关 键 词：高效液相色谱-串联质谱法 QUECHERS 蜂蜜 农药 兽药 

分 类 号：O657.63[理学—分析化学]