结合 QuEChERS法与液相色谱-三重四极杆复合线性离子阱质谱（ LC-Q-TRAP／MS）技术，建立了大米中205种农药残留的快速筛查确证方法。大米样品经乙腈提取，N-丙基乙二胺（PSA）、无水 MgSO4和 C18吸附剂净化后，采用多反应监测-信息关联采集-增强子离子（ MRM-IDA-EPI）扫描方式及谱库检索技术，通过对化合物的保留时间、离子对以及高灵敏度的 EPI谱库检索比对，完成了205种农药的筛查与确证，并采用外标法定量，实现了大米样品中205种农药的定性和定量分析。结果表明，所有农药的线性相关系数均大于0.995；方法的定量限在0.5~10.0μg／kg之间。在10、50μg／kg两个添加水平下，205种农药的平均回收率在62.4％~127.1％之间；相对标准偏差（ RSD）在1.0％~20.0％之间。该方法能够对大米样品进行实际检测，且检测时间不超过20 min。该方法快速、准确、灵敏度高，适合于大米中农药残留的快速、全面筛查和确证分析。
A method for rapid screening and confirmation of 205 pesticide residues in rice was developed by combining QuEChERS and high performance liquid chromatography-triple quadru-pole-linear ion trap mass spectrometry( LC-Q-TRAP/MS). The rice samples were extracted with acetonitrile,and then cleaned up with primary secondary amine( PSA),anhydrous mag-nesium sulfate(MgSO4)and C18 adsorbent. Finally,the samples were detected by LC-Q-TRAP/MS in multiple reaction monitoring with information-dependent acquisition of enhanced product ion( MRM-IDA-EPI)mode followed with database searching. A total of 205 pesticide residues were confirmed by retention times,ion pairs and the database searching using EPI library,and quantified by external standard method. All the pesticides showed good linearities with linear correlation coefficients all above 0. 995. The limits of quantification( LOQs)for the 205 pesti-cides were 0. 5-10. 0 μg/kg. The average recoveries of the 205 pesticides ranged from 62. 4% to 127. 1% with the relative standard deviations( RSDs ) of 1. 0% -20. 0% at spiked levels of 10μg/kg and 50 μg/kg,and only 20 min were needed for the analysis of an actual rice sample. In brief,the method is fast,accurate and highly sensitive,and is suitable for the screening and confirmation of pesticide residues in rice.
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