气相色谱-串联质谱法快速定量测定蔬果及食用菌中126种农药及代谢物残留量
Rapid Quantitative Determination of 126 Pesticides and Metabolites Residues in Vegetables, Fruits and Edible Fungi by Gas Chro-matography-tandem Mass Spectrometry Method
唐淑军 1周春梅 1梁幸 1陈怡 1宋晓仪 1宋世文 1张玲1
作者信息
- 1. 深圳市质量安全检验检测研究院,广东深圳 518101
- 折叠
摘要
[目的]建立快速定量测定蔬果及食用菌中虫螨腈等126种农药残留的气相色谱-串联质谱法.[方法]样品匀浆后,称取10.0 g样品加入10.0 mL乙腈,冷冻10 min,加入萃取盐高速振荡提取3 min,提取液用分散固相萃取净化离心后取上清液过微孔滤膜上气相色谱-串联质谱仪测定,基质匹配标准外标法定量.[结果]该方法的线性范围在0.005～0.500 mg/L,相关系数为0.9912～0.9997;定量限、低、中、高4个加标浓度,蔬菜、水果和食用菌加标回收率为81.1％～107.2％,RSD(n=6)为1.0％～12.3％.[结论]该方法的前处理方法节省检测时间和溶剂,并筛选出适合农药残留检测的高效能高寿命色谱柱(检测样品数量是通用色谱柱的3倍),大大节约成本和提高检测效率.该方法准确、快速简便、环保、经济,满足大批量实际样品的检测需求.
Abstract
[Objective]A gas chromatography-tandem mass spectrometry method was established for the rapid quantitative determination of 126 pesticide residues in vegetables, fruits and edible fungi.[Method] After homogenizing the sample, 10.0 g of the sample was weighed and 10.0 mL of acetonitrile was added.The sample was frozen for 10 minutes, and the extraction salt was added for high-speed oscillation extrac-tion for 3 minutes.The extraction solution was purified by dispersed solid-phase extraction and centrifuged.The supernatant was taken and measured by gas chromatography-tandem mass spectrometry on a microporous filter membrane.The matrix matching standard external standard method was used for quantification.[Result] The linear range of this method was 0.005-0.500 mg/L, with correlation coefficient of 0.9912-0.9997;the recovery rates of vegetables, fruits and edible mushrooms were 81.1％-107.2％ with four spiked concentrations of quantification limit, low, medium and high, and the RSD (n=6) was 1.0％-12.3％.[Conclusion] The pre-treatment method of this method saves detection time and solvents, and selects high-performance and long-life chromatography columns suitable for pesticide residue detection (the number of detection samples is three times that of general chromatography columns), greatly saving costs and improving detection effi-ciency.The method is accurate, fast, simple, environmentally friendly, and economical, meeting the testing needs of large quantities of actual samples.
关键词
气相色谱-串联质谱法/快速定量测定/蔬果/食用菌/农药残留Key words
Gas chromatography-tandem mass spectrometry method/Rapid quantitative determination/Vegetables and fruits/Edible fungi/Pesticides residues引用本文复制引用
出版年
2024
国家科技期刊平台
NSTL
万方数据