QuEChERS结合超高效液相色谱-串联质谱法同时测定畜禽肉中9种新烟碱类杀虫剂及5种代谢物残留量  

Simultaneous Determination of Nine Neonicotinoid Insecticides and Five Metabolites in Meat by QuEChERSCoupled with Ultra-high Performance Liquid Chromatography-Tandem Mass Spectrometry

作　　者：林彬彬 杨志金 黄旭良 林小莲 LIN Binbin;YANG Zhijin;HUANG Xuliang;LIN Xiaolian(Xiamen Institute for Food and Drug Quality Control,Xiamen 361013,China)

机构地区：[1]厦门市食品药品质量检验研究院,福建厦门361013

出　　处：《食品科学》2024年第24期273-281,共9页Food Science

基　　金：厦门市市场监督管理局科技项目(XMSJ202214)。

摘　　要：本研究使用QuEChERS(Quick、Easy、Cheap、Effective、Rugged、Safe)净化结合超高效液相色谱-串联质谱法建立同时测定畜禽肉中新烟碱类杀虫剂及其代谢物残留量的方法。样品经1%乙酸-乙腈提取,加入盐析剂(1 g NaCl、4 g无水MgSO_(4))盐析分层,上清液用C_(18)粉末净化后经XSelect HSS T3(150 mm×3.0 mm,2.5 μm)色谱柱进行分离,以0.1%甲酸溶液和乙腈为流动相梯度洗脱,在正离子模式下以多反应监测方式监测,采用基质匹配法进行外标定量。结果表明:9种新烟碱类杀虫剂及5 种代谢物线性关系良好,相关系数r>0.995,12种目标化合物的定量限为2 μg/kg,2种化合物的定量限为20 μg/kg,方法回收率在61.0%~116.7%之间,相对标准偏差不超过14.81%。该方法前处理步骤简便、回收率优良,可用于畜禽肉中新烟碱类杀虫剂及其代谢物的快捷、精准检测。In this study,a method for the simultaneous determination of neonicotinoid insecticides and their metabolites in meat was established by the QuEChERS(quick,easy,cheap,effective,rugged,safe)pretreatment method followed by ultra-high performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS).Samples were extracted with acetonitrile containing 1%acetic acid.After salting-out with 1 g of NaCl and 4 g of anhydrous MgSO4,the supernatant was cleaned-up using C18.The separation of the analytes was carried out on a XSelect HSS T3(150 mm×3.0 mm,2.5μm)column by gradient elution with a mobile phase composed of 0.1%formic acid and acetonitrile.The analytes were detected by multiple reaction monitoring(MRM)in the positive ion mode and quantified by the matrix-matched external standard method.The results showed that the calibration curves for all analytes had a good linearity with correlation coefficients(r)more than 0.995.The limit of quantitation(LOQ)was 2μg/kg for 12 target compounds and 20μg/kg for the two compounds.The recovery rates of the proposed method were in the range of 61.0%–116.7%with relative standard deviations(RSDs)below 14.81%.This method has the merits of simple pretreatment steps and satisfying recovery rates and enables fast and accurate detection of neonicotinoid insecticides and their metabolites in meat.

关 键 词：新烟碱类杀虫剂 代谢物 畜禽肉 QUECHERS 超高效液相色谱-串联质谱 

分 类 号：O657.63[理学—分析化学]