作　　者： (宓捷波）; (张然）; (王飞）; (许泓）; (葛宝坤）; (何佳）;

机构地区： 天津出入境检验检疫局,天津300461

出　　处： 《理化检验（化学分册）》 2017年第9期1009-1013,共5页

摘　　要： 利用在线固相萃取系统,通过萃取柱的选择和在线洗脱条件的优化,建立了测定动物源食品中阿维菌素和伊维菌素残留量的在线固相萃取-液相色谱-串联质谱法。2.50g样品经5mL乙腈和5mL的0.15%(体积分数)三乙胺溶液提取,采用HySphere C_(18) HD固相萃取柱对提取液进行在线净化。分析物经ZORBAX SB-C_(18)色谱柱(2.1mm×15mm,1.8μm)分离,采用乙腈和含0.2%(体积分数)甲酸的10mmol·L^(-1)乙酸铵溶液进行梯度洗脱。质谱分析采用电喷雾正离子源和多反应监测模式。阿维菌素和伊维菌素的质量浓度在10μg·L^(-1)内与峰面积呈线性关系,测定下限(10S/N)均为5.0μg·kg^(-1)。在猪肉、牛肉和香肠样品中进行加标回收试验,阿维菌素和伊维菌素的加标回收率在74.8%~96.5%之间,测定值的相对标准偏差(n=6)不大于11%。 A method of LC-MS/MS coupled with online solid phase extraction （SPE） for detemination of avermectin and ivermectin residues in animal origin foods was established by selection of SPE column and optimization of online eluting condition.The sample（2.50g）was extracted with 5mL of acetonitrile and 5mL of 0.15%（φ） triethanolamine solution,and the extract was purified by online clean-up with HySphere C（18） SPE column.The analytes were separated on ZORBAX SB C（18） column （2.1mm×15mm,1.8μm）with acetonitrile and 10mmol·L^-1 ammonium acetate solution containing 0.2%（φ） formic acid as mobile phase in gradient elution.ESI＋and MRM were adopted in MS analysis.Linear relationships were found between the peak areas and the mass concentrations of avermectin and ivermectin both within 10μg·L^-1,with the same lower limits of determination of 5.0μg·kg^-1.Test for recovery were made by standard addition method in the samples of pork,beef and sausage,giving recovery rates ranged from 74.8% to 96.5%,with RSDs （n=6） within 11%.

关 键 词： 液相色谱 串联质谱法 在线固相萃取 阿维菌素 伊维菌素 动物源食品