QuEChERS结合高效液相色谱串联质谱检测苹果与白菜中拟除虫菊酯类杀虫剂的研究  

Determination of Pyrethroids in Apples and Cabbages by QuEChERS-HPLC-MS/MS

作　　者：郭润泽 张成龙 刘天宇[1] 王欣欣 方文雪 杨瑞琴[1] GUO Runze;ZHANG Chenglong;LIU Tianyu;WANG Xinxin;FANG Wenxue;YANG Ruiqin(School of Investigation,People's Public Security University of China,Beijing 100038,China;Institute of Forensic Science and Technology of Xinxiang Public Security Bureau,Xinxiang 453000,China)

机构地区：[1]中国人民公安大学侦查学院,北京100038 [2]新乡市公安局刑事科学技术研究所,河南新乡453000

出　　处：《中国人民公安大学学报（自然科学版）》2024年第2期30-36,共7页Journal of People’s Public Security University of China(Science and Technology)

基　　金：中国人民公安大学刑事科学技术双一流创新研究专项(2023SYL06)。

摘　　要：建立了一种苹果与白菜样品中5种拟除虫菊酯类杀虫剂的QuEChERS结合高效液相色谱串联质谱(HPLC-MS/MS)的检测方法。根据拟除虫菊酯质谱裂解规律,优化了色谱-质谱条件;考察了不同盐析剂、缓冲体系及净化剂条件下的平均回收率,优化了QuEChERS前处理方法。结果表明,该方法可在9 min内完成氯菊酯、氰戊菊酯、甲氰菊酯、溴氰菊酯、氯氰菊酯的检验,5种目标物在各自线性范围内线性关系良好(R2≥0.995),检出限(LOD)为0.05~1.0μg/kg,定量限(LOQ)为0.1~2.0μg/kg;在10、50和100μg/kg 3个添加水平下的加标回收率(RE)为81.6~103.4%,基质效应(ME)为75.9%~97.8%,日间、日内精密度在2.62%~13.20%范围内。该方法灵敏度高、线性范围宽、绿色安全,适用于苹果、白菜样品中拟除虫菊酯的常规检验与残留检测。A detection method for five pyrethroids in apple and cabbage samples was established by using QuEChERS combined with high performance liquid chromatography⁃tandem mass spectrometry(HPLCMS/MS).The conditions of chromatography⁃mass spectrum were optimized according to the mass spectro⁃metric fragmentation patterns of pyrethroids.Besides,the average recovery under different salting⁃out a⁃gents,buffering systems and purification agents were investigated,and the QuEChERS pretreatment method was optimized.The results showed that the method could complete the determination of per⁃methrin,fenvalerate,fenpropathrin,deltamethrin and cypermethrin in 9 minutes.The linear relationship between the five targets was good in their respective linear ranges(R2≥0.995),the limit of detection(LOD)was 0.05~1.0μg/kg,and the limit of quantitation(LOQ)was 0.1~2.0μg/kg.The recovery effect(RE)of the five targets under the three addition levels of 10,50 and 100μg/kg was 81.6%~103.4%and the matrix effect(ME)was 75.9%~97.8%.The intra⁃day and inter⁃day precision was in the range of 2.62%~13.20%.This method is sensitive,wide linear range,green safety,which is suit⁃able for the routine inspection and residue detection of pyrethroids in apple and cabbage samples.

关 键 词：拟除虫菊酯类杀虫剂 QUECHERS HPLC-MS/MS 果蔬 

分 类 号：D918.93[政治法律—法学]