超高效液相色谱-串联质谱法测定粮谷中阿维菌素类杀虫剂残留  

Determination of Abamectin Residues in Grain by Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry

作　　者：何红梅[1] 赵华[1] 张春荣[1] 朱亚红[1] 平立凤[1] 吴珉[1] 张昌朋[1] 蔡晓明[1] 李振[1] 

机构地区：[1]省部共建国家重点实验室培育基地“浙江省植物有害生物防控重点实验室”农业部农药残留检测重点实验室,浙江省农业科学院农产品质量标准研究所,杭州310021

出　　处：《分析化学》2013年第11期1627-1632,共6页Chinese Journal of Analytical Chemistry

基　　金：863基金项目(No.2011AA100806);青年科学基金项目(No.21007061);分析测试科技计划项目(No.2013C37085)资助

摘　　要：建立了超高效液相色谱-串联质谱法（UPLC-MS/MS）同时测定糙米、小麦和玉米中阿维菌素类杀虫剂残留量的方法.样品经乙腈振荡提取后用自制的酸性氧化铝柱净化,采用梯度洗脱程序、BEH C18色谱柱分离柱、应用UPLC-MS/MS正离子扫描测定残留的3种阿维菌素类药物.进行了10,50,100和1000 μg/kg的添加回收实验,糙米、小麦、玉米中3种药物的平均回收率为87％ ～ 109％,日内相对标准偏差（RSD）为1％～8％.实验室内3种药物日间平均回收率为97％ ～ 107％,日间RSD为2％～9％.阿维菌素、伊维菌素和甲氨基阿维菌素苯甲酸盐检出限分别为0.5,0.5和0.1μg/kg,低于我国、欧盟和日本在粮谷中制定的最大残留限量值.阿维菌素和伊维菌素在2.0～64 μg/L、甲氨基阿维菌素苯甲酸盐在0.5～32 μg/L浓度范围内线性关系良好（r＞0.997）.A new analytical method has been developed for the simultaneous determination of abamectin residues such as abamectin, ivermectin and emamectin benzoate in grain. The samples of brown rice, wheat and corn were extracted with acetonitrile by an oscillator, cleaned up by acid alumina column, and analyzed by gradient ultra performance liquid chromatography-tandem mass spectrometry with eleetrospray ionization in positive mode （ESI＋） using a UPLC BEH C18 Column. The method was validated using fortified brown rice, wheat and corn. Mean recoveries of grain at four spiked levels （ 10, 50, 100.0 and 1000 μg/kg） were found between 87% and 109% with good precision （ RSD〈8% ） for brown rice, wheat and corn. Mean recovery of within-laboratory reproducibility was between 97% and 107% with good precision （ RSD 〈9% ） for all the pesticides at the spiked level of 50 μg/kg. Limits of detection （LODs） for abameetin, ivermectin and emamectin benzoate in brown rice, wheat and corn were 0.5, 0.5 and 0.1 μg/kg, which are lower than the maximum residue limit （MRL） established by Chinese, Japanese and European legislation in linear relationships were obtained in the range of 2.0-64μg/L for abamectin and ivermectin, and of 0.5-32μg/L for emamectin benzoate with the correlation coefficient over 0. 997. grain. Good in the range

关 键 词：阿维菌素类杀虫剂 液相色谱-串联质谱 粮谷 

分 类 号：TS210.7[轻工技术与工程—粮食、油脂及植物蛋白工程] O657.63[轻工技术与工程—食品科学与工程]