UPLC-MS/MS法同时测定蔬菜中11种有机磷和10种新烟碱类杀虫剂  

Simultaneous determination of eleven organophosphorus and ten neonicotinoid pesticide in vegetables by UPLC-MS/MS

作　　者：张艳[1] 曲良娇 凌莉[1] 张彩虹[1] ZHANG Yan;QU Liang-jiao;LING Li;ZHANG Cai-hong(Department of Physical and chemical Test,Zhuhai Center for Disease Control and Prevention,Zhuhai,Guangdong 519060,China)

机构地区：[1]珠海市疾病预防控制中心理化检验所,广东珠海519060

出　　处：《现代预防医学》2024年第4期722-727,共6页Modern Preventive Medicine

基　　金：珠海市社会发展领域科技计划项目(2220004000115)。

摘　　要：目的 建立同时测定蔬菜中11种有机磷和10种新烟碱类杀虫剂的超高效液相色谱-串联质谱法(UPLC-MS/MS)。方法 样品用乙腈提取,经无水硫酸镁、PSA和C18净化,采用HSS T3色谱柱分离。在正离子多反应监测模式下检测,基质匹配标准曲线外标法定量。结果 21种杀虫剂在0.50~100 ng/ml范围内相关系数大于0.999。21种杀虫剂的平均回收率为76.0%~119.3%,相对标准偏差小于10%,方法检出限为0.02~1.7μg/kg,定量限为0.06~5.7μg/kg。对从市场采集的76份蔬菜进行检测,在26份蔬菜中检出了9种目标组分,浓度在0.012~3.16 mg/kg之间。结论 该方法简便、灵敏、准确,适用于蔬菜中有机磷和新烟碱类杀虫剂的检测。Objective eTo develop an ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)method for the determination of eleven organophosphorus and ten neonicotinoid pesticides in vegetables.Methods Pesticides in sample were extracted with acetonitrile,cleaned up using a sorbent mixture of magnesium sulfate anhydrous,PSA and Cis.The separation was performed on a HSS T3 column.Detection was operated on multiple reaction monitoring scan under positive electrospray ionization.Matrix-matched external standard calibration curves were used for quantification.Results The linear rang of calibration curves ranged from 0.50-100 ng/ml.Good linearities(r>0.999)were obtained for all 21 pesticides.The average recoveries were 76.0%-119.3%with RSD<10%for all the analytes.The limits of detection and quantification were 0.02-1.7μg/kg and 0.06-5.7μg/kg,respectively.This method was applied to analyze 76 vegetable samples from market.Nine target pesticides were detected in 26 samples,with a contents of 0.012-3.16 mg/kg.Conclusion This method is simple,sensitive,and accurate,and it is suitable for the determination of organophosphorus and neonicotinoid pesticide residues in vegetables.

关 键 词：有机磷 新烟碱类杀虫剂 蔬菜 QUECHERS UPLC-MS/MS 

分 类 号：R115[医药卫生—公共卫生与预防医学]