气相色谱-负化学源质谱法测定禽蛋及蛋制品中氟虫腈及其代谢物  

Determination of fipronil and its metabolites in eggs and egg products with gas chromatography-negative chemical ionization-mass spectrometry

作　　者：沈伟健[1] 柳菡[1] 张睿[1] 余可垚[1] 蔡理胜 刘艳[1] 王红 Shen Weijian;Liu Han;Zhang Rui;Yu Keyao;Cai Lisheng;Liu Yan;Wang Hong(Food Laboratory of Jiangsu Entry-Exit Inspection and Quarantine Bureau,Nanjing 210019,China)

机构地区：[1]江苏出入境检验检疫局食品实验室,江苏南京210019

出　　处：《色谱》2017年第12期1224-1228,共5页Chinese Journal of Chromatography

基　　金：基金项目 国家认证认可监督管理委员会行业标准紧急制定任务(2017B261j)~~

摘　　要：建立了气相色谱-负化学源质谱联用技术(GC-NCI-MS)测定禽蛋及蛋制品中氟虫腈及其3种代谢物残留量的方法。样品经乙腈提取,分散固相萃取技术QuEChERS净化,采用基质校正曲线外标法定量。在0.005~0.10mg/L范围内氟虫腈及其3种代谢物均呈现良好的线性关系,所有目标物的定量限均在0.025~0.10μg/kg范围内,均能满足国内外的限量要求。在0.1、2.0、4.0、20.0μg/kg 4个添加水平下,氟虫腈及其3种代谢物的平均回收率均处于87.0%~99.3%,RSD均≤12.7%,说明该法有较高的准确度和较好的稳定性。综上所述,该法灵敏度、准确度较高,精密度较好,可用于禽蛋及蛋制品中氟虫腈及其代谢物残留量的测定。A method was established for the determination of fipronil and its metabolites in eggs and egg products with gas chromatography-negative chemical ionization-mass spectrometry(GC-NCI-MS).The targets were extracted from samples with acetonitrile,and followed by a simple cleanup step known as dispersive solid-phase extraction QuEChERS.The extracts were determined by GC-NCI-MS,and quantified by external standard method with matrix correction standard curves.The recoveries were in the range of87.0%to99.3%at four spiked levels(0.1,2.0,4.0and20.0p^^k g),and all RSDs were not more than12.7%for the four analytes.The linearity of the method was good between0.005and0.10mg/L,and all LOQs were less than0.10pg/kg.So this method can be used to determine the residues of fipronil and its metabolitesin eggs and egg products.

关 键 词：QUECHERS 气相色谱-质谱 负化学源 氟虫腈及其代谢物 禽蛋 蛋制品 

分 类 号：O658[理学—分析化学]