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食品研究与开发:2025,46(9):178-187
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QuEChERS-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
(1.沈阳市食品药品检验所,辽宁 沈阳 110124;2.辽宁省检验检测认证中心,辽宁 沈阳 110036)
Quick Detection of Pesticides Residues in Fruits by QuEChERS-High-performance Liquid Chromatography-Triple Quadrupole Linear Ion Trap Mass Spectrometry
(1. Shenyang Food and Drug Inspection Institute, Shenyang 110124, Liaoning, China;2. Liaoning Inspection, Examination & Certification Centre, Shengyang 110036, Liaoning, China)
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投稿时间:2023-09-06    
中文摘要: 为建立水果中17 种杀虫剂高效液相色谱串联质谱(high-performance liquid chromatography tandem mass spectrometry,HPLC-MS/MS)的快速检测方法,在样品中加入1 g 柠檬酸钠二水合物、0.5 g 柠檬酸二钠盐倍半水合物,加入10 mL 乙腈,取上清液经过0.4 g 无水硫酸镁、0.3 g 乙二胺-N-丙基硅烷化硅胶、0.01 g 石墨化碳黑和0.2 g HCC18 超洁净填料净化处理,在多反应监测(multiple reaction monitoring,MRM)→信息依赖性采集(information dependent acquisition,IDA)→增强子离子扫描(enhanced ion scanning,EPI)模式下进行检测,结果通过二级全扫描质谱图和数据处理软件进行解析。经实际样品检测确定,该方法可筛选和定性目标及非目标代谢产物,提高检测效率,适合用于对水果中17 种杀虫剂的检测。
Abstract:A quick detection method was established for 17 pesticides in fruits by high-performance liquid chromatography tandem mass spectrometry (HPLC-MS/MS). 1 g of sodium citrate dihydrate, 0.5 g of sodium citrate sesquihydrate, and 10 mL of acetonitrile were added to the sample. The supernatant was taken and purified with 0.4 g of anhydrous magnesium sulfate, 0.3 g of ethylenediamine-N-propylsilylated silica gel (PSA),0.01 g of graphitized carbon black (GCB), and 0.2 g of HC-C18 ultra clean filler. Detection was performed in multiple reaction monitoring(MRM) → information dependent acquisition (IDA) → enhanced ion scanning(EPI) mode. The results were analyzed with second-order full-scan mass spectrometry and data processing software. After actual sample testing, it had been determined that this method can screen and characterize the target and non-target metabolites to improve the detection efficiency. It was suitable for the detection of 17 pesticides in fruits.
文章编号:202509023     中图分类号:    文献标志码:
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)
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