分散固相萃取-UHPLC-APCI-MS/MS测定猪肉中阿维菌素药物残留量  

Determination of abamectin residue in pork by dispersive solid-phase extraction UHPLC-APCI-MS/MS

作　　者：高玉玲 孙鹏[1,2] 梁婷 郭永霞[1] GAO Yu-ling;SUN Peng;LIANG Ting;GUO Yong-xia(Testing Center,Heilongjiang Bayi Agricultural University,Daqing 163319,China;Test Center of Quality Supervision and Inspection of Processed Agriculmral Products in Ministry of Agriculture and Rural Affairs of the Pepple's,Heilongjiang Bayi Agricultural University,Daqing 163319,China;Agricultural and Rural Area Bureau of Daiyue District Taian'City,Taian 271000,China)

机构地区：[1]黑龙江八一农垦大学测试中心,黑龙江大庆163319 [2]黑龙江八一农垦大学农业农村部农产品及加工品质量监督检验测试中心(大庆),黑龙江大庆163319 [3]泰安市岱岳区农业农村局,山东泰安271000

出　　处：《高师理科学刊》2019年第7期64-68,共5页Journal of Science of Teachers＇College and University

基　　金：大庆市指导性科技计划项目(zd-2017-80)

摘　　要：建立了分散固相萃取-超高效液相色谱-大气压电离串联质谱(UHPLC-APCI-MS/MS)法测定猪肉中阿维菌素残留量的检测方法.样品经乙腈提取,N-丙基乙二胺吸附剂(PSA)和十八烷基键合硅胶吸附剂(C18)分散固相萃取吸附剂净化,优化了流动相比例、柱温、流速、碎裂电压、碰撞能及吸附剂用量、吸附剂种类对结果的影响,采用多反应监测(MRM)模式进行分析.结果表明,阿维菌素在5~500μg·L^-1范围内保持良好线性关系,线性相关系数为0.9995,在2,5,10μgkg^-1加标水平下,平均回收率在89.6%~98.4%,RSD为5.3%~8.4%;检出限为1.2μg·kg^-1,定量限为4.2μg·kg^-1.该方法操作简单,结果准确,有机试剂使用量小,可满足肉制品中阿维菌素药物残留检测的需要.A new analytical method has been developed for determination of abamectin residues in pork by dispersive solid-phase extraction combined with UHPLC-APCI-MS/MS.The sample was extracted with acetonitrile and primarily purified by dispersive solid phase extraction with primary secondary amine(PSA)and octadecyl bonded silica(C18)as absorbent,the effects of experimental factors on mobile phase proportion,column temperature,flow velocity,fragmentor,collision energy,the kinds and dose of adsorbents for experimental results were optimized.The sample was analyzed with multiple reaction monitoring mode(MRM). It was shown that good linearity was obtained at concentrations of 5.0 to 500.0 μg·L^-1 and the correlation coefficient is 0.999 5 for abamectin,the average recovery of abamectin in pork is 89.6%~98.4% at spiked levels of 2,5,10 μg kg^-1,the relative standard deviation is 5.3%~8.4%(n=6),the limits of detection(LOD)and limits of quantification(LOQ)for abamectin were 1.2 μg·kg^-1 and 4.2 μg·kg^-1 respectively.The proposed method is simple,accurate,little reagent-consuming and it could meet the requirements for the determination of abamectin residue.

关 键 词：分散固相萃取 超高效液相色谱串联质谱 阿维菌素 猪肉 

分 类 号：O657[理学—分析化学]