气相色谱/离子阱质谱-选择离子方法同时检测大米中百种农药残留

Multi-residue Method for Simultaneous Analysis of 107 Pesticides in Rice by Gas Chromatography/Mass Spectrometry

建立了一种以气相色谱/离子阱质谱（GC/MS）,选择离子技术为基础的多种农药同时检测方法.净化采用凝胶渗透色谱（GPC）和Florisil小柱.通过GC/MS/SIM技术对农药进行检测,在对色谱条件,扫描离子进行优化后,前处理余留下的杂质通过检测的方法得到了进一步的去除,实现了一次进样同时对107种农药进行分析.方法准确灵敏,对于大部分农药回收率保持在70%～110%;相对标准偏差小于20%;检出限保持在0.01～0.2 mg/kg 之间（信噪比3）.

A multiresidue method is described properties pesticides in flee, the ranges including for simultaneous analysis of 107 pesticides with different organophosphorus, organochlorine, carbamate and synthetic pyrethroid pesticides. Lipids were removed using gel permeation chromatography（GPC）. Liquid chromatography-Florisil column were used for further clean up other unkown small size molecular interference. By optimizing the oven program and the selective monitor program, the interference from the clean-up procedure was further minimized and the pesticides were finally determined simultaneously using one injection. The average recoveries for most pesticides（ at the spiked level of 0.02, 0.1 and 1 μg/g） were between 70% - 110%. The relative standard deviation of the method was less than 20% for each case, and the limit of detection （.LOD） was defined in terms of 3 times baseline noise, varied from 0. 01 to 0. 2 mg/kg, depending on the compound.