QuEChERS-气相色谱-串联质谱法测定食用花卉中7种常见杀虫剂的含量  

Determination of 7 Common Insecticides in Edible Flowers by Gas Chromatography-Tandem Mass Spectrometry with QuEChERS

作　　者：徐倩[1] 孙志洪 路瑞娟 郭伟伟 倪洁 XU Qian;SUN Zhihong;LU Ruijuan;GUO Weiwei;NI Jie(Hebei Cangzhou Center for Disease Control and Prevention,Cangzhou 061000,China;Hebei Cangzhou Ecological Environment Monitoring Center,Cangzhou 061000,China;Cangzhou Academy of Ecological and Environmental Protection,Cangzhou 061000,China;Cangzhou Ecological Environment Monitoring Center,Cangzhou 161000,China;Hebei Hengshui Ecological Environment Monitoring Center,Hengshui 053000,China)

机构地区：[1]河北省沧州市疾病预防控制中心,沧州061000 [2]河北省沧州生态环境监测中心,沧州061000 [3]沧州市生态环境保护科学研究院,沧州061000 [4]沧州市生态环境保护科学研究院,061005 [5]河北省衡水生态环境监测中心,衡水053000

出　　处：《理化检验（化学分册）》2024年第2期222-226,共5页Physical Testing and Chemical Analysis(Part B:Chemical Analysis)

摘　　要：提出了QuEChERS自动样品制备系统提取、净化,气相色谱-串联质谱法测定食用花卉中三氯杀螨醇、腈菌唑、对甲抑菌灵、环氟菌胺、抗蚜威、杀螟硫磷和啶虫丙醚等7种杀虫剂含量的方法。在10 g食用花卉样品中加入20 mL乙腈和一个萃取包(4 g无水硫酸镁、1 g氯化钠、1 g柠檬酸钠、0.5 g柠檬酸二钠)。振摇后加入净化剂(500 mg硫酸镁、150 mg N-丙基乙二胺和15 mg石墨化碳黑),按照程序进行自动提取、净化。离心,上清液氮吹至近干,用丙酮溶解残留物。溶液中的目标物用Rtx-5MS色谱柱在程序升温条件下分离,电子轰击离子源电离,多反应监测模式检测。结果显示:7种杀虫剂的质量浓度在0.005~5.0 mg·L^(-1)内和峰面积呈线性关系,测定下限(10S/N)为0.0076~0.029 mg·kg^(-1);按照标准加入法进行回收试验,回收率为83.2%~116%,测定值的相对标准偏差(n=6)小于5.0%。方法用于9批食用花卉样品的分析,三氯杀螨醇检出率较高,仅有一批样品中的检出量(0.013 mg·kg^(-1))超过其测定下限(0.0076mg·kg^(-1))。The QuEChERS automatic sample preparation system was used for extraction and purification,and gas chromatography-tandem mass spectrometry was proposed to determine the 7 insecticides in edible flowers,including dicofol,myclobutanil,tdyfluanid,cyflutenamid,pirimicarb,fenitrothion and pyridalyl.Acetonitrile(20 mL)and an extraction package(4 g of anhydrous magnesium sulfate,1 g of sodium chloride,1 g of sodium citrate,and 0.5 g of disodium citrate)were added into 10 g of edible flower sample.After shaking,purification agents(500 mg of magnesium sulfate,150 mg of N-propylethylenediamine,and 15 mg of graphitized carbon black)were added,and automatic extraction and purification were performed according to the program.The mixture was centrifuged,and the supernatant was blown to near dryness by nitrogen.The residue was dissolved by acetone,and targets in the resulting solution was separated using the Rtx-5MS chromatographic column under programmed heating conditions,ionized by electron impact ion source,and detected using the multiple reaction monitoring mode.It was shown that linear relationships between values of the mass concentration and the peak area of the 7 insecticides were kept in the range of 0.005-5.0 mg·mL^(-1),with lower limits of determination(10S/N)in the range of 0.0076-0.029 mg·kg^(-1).Test for recovery was made according to the standard addition method,giving recoveries in the range of 83.2%-116%,and RSDs(n=6)of the determined values were less than 5.0%.The proposed method was used for the analysis of 9 batches of edible flower samples,and the detection rate of dicofol was relatively high,with detection amount(0.013 mg·kg^(-1))of dicofol in only one batch of sample exceeding its lower limit of determination(0.0076 mg·kg^(-1)).

关 键 词：QUECHERS 气相色谱-串联质谱法 杀虫剂 食用花卉 

分 类 号：O657.63[理学—分析化学]