高效液相色谱-三重四极杆复合离子阱质谱法快速检测水果中杀虫剂残留
Determitation of pesticide residues in fruits by high performance liquid chromatography-triple quadrupole-ion trap mass spectrometry
罗景阳 1袁帅 1关健 2李巧莲 1王岩松 1刘鑫1
作者信息
- 1. 沈阳市食品药品检验所,沈阳 110124
- 2. 辽宁省检验检测认证中心,沈阳 110036
- 折叠
摘要
[目的]通过优化QuEChERS法结合高效液相色谱-三重四极杆复合离子阱质谱,建立水果中17种杀虫剂快速检测方法.[方法]样品通过10 mL乙腈和提取盐(4g无水硫酸镁、1g氯化钠,1g柠檬酸钠二水合物、0.5g柠檬酸二钠盐倍半水合物)溶剂萃取,再经过300 mg乙二胺-N-丙基硅烷化硅胶(PSA)、10 mg石墨化炭黑(GCB)、200 mg十八烷基硅烷键合硅胶(C18)和1000mg无水硫酸镁净化处理,采用多反应监测-信息依赖性采集-增强子离子扫描的采集扫描模式(MRM-IDA-EPI)进行检测,建立EPI数据谱库.检测结果通过保留时间、离子对峰度比及数据库EPI谱图对比进行定性,采用基质匹配外标法定量.[结果]化合物的线性范围分别为0.5～25 μg/L或2～50 μg/L,决定系数R2≥0.990 13,检出限为0.5～2 μg/kg,定量限为1～5 μg/kg,样品的加标回收率为70.69％～117.40％,精密度为0.82％～13.81％.[结论]该方法操作简便、快速,准确性好,适用于水果中多种杀虫剂残留量的检测.
Abstract
[Aims]This article established a rapid detection method for 17 pesticides in fruits by combining QuEChERS purification method with high-performance liquid chromatography-triple quadrupole-ion trap mass spectrometry.[Methods]The samples were extracted with 10 mL acetonitrile and extraction salt(MgSO4 4 g,sodium chloride 1 g,sodium citrate dihydrate 1 g,disodium citrate sesquihydrate 0.5 g).The extract was further purified using 300 mg of primary secondary amine(PSA),10 mg of graphitized carbon black(GCB),200 mg of ostade-cylsilane(C18)and 1000 mg of MgSO4.The samples were analyzed using MRM-IDA-EPI mode,and an EPI database was established.Qualitative analysis was performed based on retention time,ion pair peak ratio,and EPI database,and quantification was carried out using matrix-matched external standard method.[Results]The linear ranges of the compounds were 0.5-25 or 2-50 μg/L,and coefficients of determination R2≥0.990 13.The limits of detection ranged from 0.5 to 2 μg/kg and the limits of quantification ranged from 1 to 5 μg/kg.The spiked recoveries of the samples were between 70.69％and 117.40％,and the precision was in the range of 0.82％to 13.81％.[Conclusions]This method was simple,fast,accurate,and suitable for the detection of various pesticide residues in fruits.
关键词
杀虫剂/高效液相色谱-三重四极杆复合离子阱质谱/水果/QuEChERSKey words
insecticide/high-performance liquid chromatography-triple quadrupole-ion trap mass spectrometry/fruit/QuEChERS引用本文复制引用
基金项目
辽宁省市场监督管理局科技计划项目(2022ZC023)
沈阳市科技计划项目(22-322-3-37)
出版年
2024
NETL
NSTL
维普
万方数据