分散固相萃取-高效液相色谱-串联质谱法测定饲料中氯虫苯甲酰胺残留量  

Determination of Chlorantraniliprole Residues in Feeds by High Performance Liquid Chromatography-Tandem Mass Spectrometry After Dispersive Solid Phase Extraction

作　　者：魏云计 何正和 李瑞阳 朱臻怡 姜颖慧 陆井莲 何健 冯民 WEI Yunji;HE Zhenghe;LI Ruiyang;ZHU Zhenyi;JIANG Yinghui;LU Jinglian;HE Jian;FENG Min(State Key Laboratory of Feed Safety Testing(Huai’an),Huai’an Customs,Huai’an 223001)

机构地区：[1]国家饲料安全检测重点实验室(淮安),淮安海关,江苏淮安223001

出　　处：《分析科学学报》2021年第6期851-854,共4页Journal of Analytical Science

基　　金：南京海关科研项目(No.2019KJ17);江苏检验检疫局科研项目(No.2018KJ11)。

摘　　要：本文建立了分散固相萃取-高效液相色谱-串联质谱测定饲料中氯虫苯甲酰胺残留的分析方法。样品采用乙酸乙酯-丙酮(7∶3,V/V)混合溶剂提取,分散固相萃取填料N-丙基乙二胺(PSA)净化,Agilent Zorbax SB-C18色谱柱分离,以甲醇和5 mmol/L NH_(4)Ac溶液(含0.1%甲酸)为流动相,梯度洗脱;质谱采用电喷雾电离,以多反应监测模式(MRM)检测,外标法定量。本方法回收率范围为70.0%~93.0%,相对标准偏差在6.1%~11.7%范围;检测限为5.0μg/kg,定量限为10.0μg/kg。A method was developed for the determination of chlorantraniliprole in feeds by high performance liquid chromatography-tandem mass spectrometry.The samples were extracted with ethyl acetate-acetone(70∶30,V/V)mixed solvent,purified by dispersive solid phase extraction primary secondary amine(PSA),and separated on Agilent Zorbax SB-C18 column by gradiently elution with methanol and 5 mmol/L ammonium acetate solution(containing 0.1% formic acid)as mobile phases.The target compound was detected by electrospray ionization with multiple reaction monitoring mode and quantified by external standard method.This method is rapid,simple and efficient.Average recoveries were between 70.0% and 93.0% with relative standard deviations between 6.1% and 11.7%.The limit of detection was 5.0 μg/kg,and limit of quantitation was 10.0 μg/kg.

关 键 词：高效液相色谱-串联质谱 饲料 氯虫苯甲酰胺 分散固相萃取 

分 类 号：O657.63[理学—分析化学]