加压流体提取-多壁碳纳米管净化-气质联用法测定温室种植土壤中烯啶虫胺、呋虫胺等7种常用烟碱类杀虫剂残留  

Determination of residues of 7 commonly used nicotinic insecticides in greenhouse soil by pressure fluid extraction,multi-wall carbon nanotube purification on GC-MS/MS

作　　者：张正 蒋幸幸 ZHANG Zheng;JIANG Xing-xing(Henan Nanyang Ecological Environment Monitoring Center,Nanyang 473000)

机构地区：[1]河南省南阳生态环境监测中心,河南南阳473000

出　　处：《化学研究与应用》2025年第2期459-464,共6页Chemical Research and Application

摘　　要：建立加压流体提取-多壁碳纳米管净化-气质联用法监测温室种植土壤中7种常用烟碱类杀虫剂(烯啶虫胺、呋虫胺、噻虫嗪、噻虫胺、噻虫啉、吡虫啉和唑虫酰胺)微量残留检测方法。称取10 g预处理后的样品至加压流体提取池中,以丙酮/二氯甲烷混合溶剂(V:V,1:1)为萃取溶剂进行提取,多壁碳纳米管净化,净化液经Rtx-5ms型石英毛细管色谱柱分离后,气质联用仪检测。7种杀虫剂质量浓度在0.02~2.0μg·mL-1范围内与对应的定量离子峰面积呈良好的线性关系。检出限在0.005~0.008 mg·kg^(-1);方法回收率平均值在85.6~109.3%之间;方法精密度范围为1.49~3.14%。实验建立的方法具有操作简单,净化效果好,定性定量检测结果准确等优点。To establish a method for determination of residues of 7 commonly used nicotinic insecticides(endinium,furotestamine,thiamethoxam,thiamethoxam,thiacloprid,imidacloprid and zolacidamide)in greenhouse soil by pressurized fluid extraction,multiwall carbon nanotube purification on GC-MS/MS.10g Pre-treated sample was weighed into a pressurized fluid extraction tank,and extracted with acetone/dichloromethane mixed solvent(V:V,1:1).Samples were purified by multi-wall carbon nanotubes,separated by Rtx-5ms quartz capillary column and detected on GC-MS/MS.External standard was selected for quantitative analysis.The mass concentration of 7 nicotinic fungicides in the range of 0.02~2.0μg:mL-'showed a good linear relationship with the corresponding quantitative ion peak area.The detection limit is 0.005~0.008 mg·kg^(-1),and average recovery rate was 85.6~109.3%.The precision RSDS(n=6)were in the range of 1.49~3.14%.The method established in the experiment has the advantages of simple operation,good purification effect,and accurate qualitative and quantitative detection results.

关 键 词：加压流体提取 GC-MS/MS 温室土壤 烯啶虫胺 烟碱类杀虫剂 

分 类 号：O657.7[理学—分析化学]