固相萃取净化结合液相色谱-串联质谱法测定禽蛋中5种阿维菌素类化合物  

Determination of five avermectins in eggs by liquid chromatography-tandem mass spectrometry combined with solid-phase extraction

作　　者：赵志勇[1] 张艳梅 鄂恒超 陈磊[1] 赵晓燕[1] 周昌艳[1] ZHAO Zhiyong;ZHANG Yanmei;E Hengchao;CHEN Lei;ZHAO Xiaoyan;ZHOU Changyan(Institute for Agro-food Standards and Testing Technology,Shanghai Academy of Agricultural Sciences,Shanghai 201403,China)

机构地区：[1]上海市农业科学院农产品质量标准与检测技术研究所,上海201403

出　　处：《分析试验室》2022年第6期720-725,共6页Chinese Journal of Analysis Laboratory

基　　金：农村农业部农业行业标准制修订项目(181821301092372035)资助。

摘　　要：建立了同时测定禽蛋中(鸡蛋、鸭蛋和鹅蛋)阿维菌素、伊维菌素、多拉菌素、乙酰氨基阿维菌素、莫西菌素等药物残留的液相色谱-串联质谱法(LC-MS/MS)。禽蛋样品采用1%甲酸乙腈溶液提取并盐析分层,上清液经Oasis PRiME HLB小柱净化。以0.1%甲酸乙腈溶液和含10 mmol/L乙酸铵的0.1%甲酸水溶液为流动相,采用ACQUITY UPLC BEH C_(18)色谱柱进行分离,质谱法在正离子模式下检测,外标法定量。结果表明5种目标物在0.1~250μg/L范围内呈现良好的线性,相关系数(R^(2))>0.99。莫西菌素在禽蛋中的定量限(LOQ)为1.0μg/kg,其他药物定量限为0.5μg/kg,回收率79%~108%,相对标准偏差(RSD)为1.2%~9.3%。同时发现,质谱气帘气压力是影响阿维菌素类药物灵敏度的关键因素。该方法能够满足禽蛋中5种阿维菌素类药物同时检测的要求。A liquid chromatography-tandem mass spectrometric(LC-MS/MS) method was developed for simultaneous determination of abamectin,ivermectin,doramectin,eprinomectin and moxidectin in poultry eggs(chicken egg,duck egg and goose egg).The sample was extracted by acetonitrile containing 1% formic acid.After salting-out,the supernatant was purified with Oasis PRiME HLB.The extract was separated on ACQUITY UPLC BEH C_(18) and detected on mass spectrometry in positive mode,quantified by external standard method.Good linearities of five avermectins were shown in the range of 0.1-250 μg/L with correlation coefficients(R~2)greater than 0.99.The limits of quantitation(LOQs)of moxidectin and other four avermectins in eggs were1.0 μg/kg and 0.5 μg/kg,respectively.Recovery of avermecins ranged from 79% to 108%,with the relative standard deviations of 1.2%-9.3%.It was also found that the gas curtain pressure was the key factor affecting the sensitivity of avermectin drugs.The method could meet the requirements for simultaneous determination of five avermectins in eggs with simplicity,high sensitivity and good reproducibility.

关 键 词：阿维菌素类 禽蛋 固相萃取 液相色谱串联质谱法 

分 类 号：O657.63[理学—分析化学] TS207.5[理学—化学]