固相萃取-三重串联四极杆气相色谱/质谱联用分析韭菜中8种氨基甲酸酯农药残留  

Analysis of 8 carbamate pesticide residues in chive using solid-phase extraction and gas chromatography-triple quadrupole mass spectrometry

作　　者：金永高[1] 范建中[1] 李继革[1] 王玉飞[1] 周静峰[2] 施家威[1] 

机构地区：[1]宁波市疾病预防控制中心宁波市毒物研究与控制重点实验室,浙江宁波315010 [2]浙江医药高等专科学校,浙江宁波315000

出　　处：《中国卫生检验杂志》2013年第2期297-300,共4页Chinese Journal of Health Laboratory Technology

摘　　要：目的:建立了韭菜中8种氨基甲酸酯农药残留的三重串联四极杆气相色谱/质谱联用分析方法。方法:样品用乙腈匀浆提取后采用固相萃取法(SPE)净化,采用三重串联四极杆气相色谱/质谱联用在多反应监测模式(MRM)下进行测定,外标法定量。结果:分别对韭菜进行两个水平的加标回收试验(50μg/kg、200μg/kg),其回收率在94.5%～106.3%范围,方法的相对标准偏差小于8%,方法的定量下限(LOQ)范围为0.8μg/kg～8.7μg/kg。结论:该方法适合韭菜中8种氨基甲酸酯农药残留的测定,具有良好的回收率及稳定性。Objective：A new method was developed and validated for the simultaneous analysis of the 8 carba- mate pesticide residues in chive by gas chromatography coupled with triple quadrupole mass spectrometry （GC - QqQ- MS/MS）. Methods： The samples were extracted with acetonitrile, and cleaned up by solid- phase extrac- tion （SPE）. The extracts were analyzed by gas chromatography coupled with triple quadrupole mass spectrometry （GC -QqQ- MS/MS） using external standard method. Results： The recoveries determined at two spiked levels of 50 μg/kg, and 200 μg/kg ranged from 94.5% to 106.3%. The RSDs were less than 8%. The limits of quantifica- tion （LOQs） were between 0.8 μg/kg to 8.7 μg/kg （Signal/Noise is 10）. Conclusion： The method can be ap- plied to the routine analysis of the 8 carbamate pesticide residues in chive.

关 键 词：三重四极杆气相色谱 质谱联用 固相萃取 农药残留 

分 类 号：O657.63[理学—分析化学]