QuEChERS-高效液相色谱串联质谱法检测鸡蛋中金刚烷胺、金刚乙胺、氟虫腈及其代谢物残留  

Determination of Amantadine,Rimantadine,Fipronil and Their Metabolites in Eggs by QuEChERS-HPLC-MS/MS Method

作　　者：欧阳小艳 黄珊[1] 蒙德军 韦卓才 覃沛 OUYANG Xiaoyan;HUANG Shan;MENG Dejun;WEI Zhuocai;Qin Pei(Nanning Municipal Center For Disease Control and Prevention,Nanning 530023,China;Guangxi Research Institute of Chemical Industry,Nanning 530001,China)

机构地区：[1]南宁市疾病预防控制中心,广西南宁530023 [2]广西化工研究院有限公司,广西南宁530001

出　　处：《化工技术与开发》2024年第6期62-66,共5页Technology & Development of Chemical Industry

基　　金：广西壮族自治区卫生健康委员会自筹科研项目(Z-A20221263)。

摘　　要：建立了采用QuEChERS结合高效液相色谱-串联质谱法,快速测定鸡蛋中的金刚烷胺、金刚乙胺、氟虫腈及其代谢物残留量的方法。鸡蛋样品经水^(-1)%甲酸乙腈涡旋提取、盐析、QuEChERS净化后,以A Venusil MP C18色谱柱为分析柱,0.1%甲酸水-乙腈为流动相,进行梯度洗脱,采用正负离子喷雾模式电离,多反应离子监测方式进行定性及定量分析。在0.1~20.0ng·mL^(-1)的线性范围内,6种化合物的回归方程均呈良好的线性关系,相关系数r>0.9995。金刚烷胺、金刚乙胺、氟虫腈、氟虫腈砜、氟虫腈亚砜、氟甲腈的检出限,分别为0.5、0.5、0.1、0.1、0.1、0.1μg·kg^(-1),在低、中、高3组浓度水平下,平均加标回收率在81.1%~113.0%之间,相对标准偏差(RSD)在0.2%~9.2%之间。该方法的前处理简单易操作,检测速度快,检测灵敏度和准确度高,重现性好,可以满足同时快速检测鸡蛋中金刚烷胺、金刚乙胺、氟虫腈及其代谢产物残留的需求。A method for the rapid determination of amantadine,rimantadine,fipronil and their metabolites in eggs by QuEChERSHPLC-MS/MS was established.The egg samples were extracted by vortex with water and 1% formic acid acetonitrile,salted and purified by QuEChERS.The analytical column was A Venusil MP C18,the mobile phase was 0.1% formic acid acetonitrile solution,the ionization mode was positive and negative ion spray mode,and the qualitative and quantitative detection was performed by multireaction ion monitoring pattern.The regression equations of the six compounds showed good linearity in the linear range of 0.1~20.0ng/mL with correlation coefficient r>0.9995.The detection limits of amantadine,rimantadine,fipronil,fipronil sulfone,fipronil sulfoxide and fipronil desulfinyl were 0.5,0.5,0.1,0.1,0.1,0.1 μg/kg,respectively.At the low,middle and high concentration levels,the average recoveries were 81.1%~113.0%,and the relative standard deviation(RSD) were 0.2%~9.2%.The method had the advantages of simple pretreatment,rapid detection,high sensitivity and accuracy,and good reproducibility.

关 键 词：QUECHERS 鸡蛋 金刚烷胺 金刚乙胺 氟虫腈及其代谢物 高效液相色谱-串联质谱法 

分 类 号：O657.63[理学—分析化学]