QuEChERS-超高效液相色谱-电喷雾串联质谱法测定小麦籽粒、植株和土壤中氯啶菌酯残留  

Determination of Triclopyricarb Residues in Wheat Grain,Straw and Soil by QuEChERS-High Performance Liquid Chromatography-Triple Quadrupole Tandem Mass Spectrometry

作　　者：魏进 张盈 李汶锟 秦立新 段婷婷 

机构地区：[1]贵州省植物保护研究所,贵州贵阳550006

出　　处：《山东农业科学》2016年第4期124-128,共5页Shandong Agricultural Sciences

基　　金：贵州省农业科技攻关项目"基于植物源酯酶筛选农药残留快速检测试纸的研制与应用"[黔科合NY字(2012)3050号]

摘　　要：建立了小麦籽粒、植株和土壤中氯啶菌酯残留的Qu ECh ERS-高效液相色谱-电喷雾串联质谱（UPLC-ESI-MS/MS）检测方法。样品用乙腈溶液提取,经Qu ECh ERS方法净化,以Hypersil GOLD色谱柱（100 mm×2.1 mm,1.9μm）进行HPLC分离,以电喷雾电离串联质谱正离子多反应监测（MRM）模式进行测定。对氯啶菌酯在小麦籽粒、植株和土壤中3个添加水平（0.01、0.10、1.00 mg·kg-1）下的回收率进行了测定,氯啶菌酯在小麦植株中的回收率为83.3%-99.7%（RSD为4.1%-5.7%）,在麦粒中的回收率为88.4%-108.7%（RSD为4.4%-7.1%）,在土壤中回收率为81.2%-98.9%（RSD为2.8%-7.1%）。该方法样品前处理简单、快速,分析时间短,灵敏度、准确度和精密度均符合农药残留检测要求,适用于小麦籽粒、植株和土壤中氯啶菌酯残留的检测。A method was developed for the determination of triclopyricarb residues in wheat grain,straw and soil by QuEChERS- ultra performance liquid chromatography coupled with electrospray ionization tandem mass spectrometry（ UPLC- ESI- MS / MS）. The residues in the samples were extracted by acetonitrile,cleaned up by developed QuEChERS method,and then analyzed by LC- MS / MS in multiple reaction monitoring（ MRM） mode via positive electrospray ionization with an Hypersil GOLD column（ 100 mm × 2. 1 mm,1. 9 μm） as the analytical column. The recoveries of triclopyricarb spiked at three levels of 0. 01,0. 10 and1. 00 mg·kg- 1were from 83. 3% to 99. 7% with the relative standard deviation（ RSD） of 4. 1% - 5. 7% in wheat straw,from 88. 4% to 108. 7% with the RSD of 4. 4% - 7. 1% in grain,from 81. 2% to 98. 9% with the RSD of 2. 8% - 7. 1% in soil. The pretreatment process of this method was simple and rapid,the analytical process was fast,and the sensitivity and accuracy all met the requirements of pesticide residue detection.So,this method was applicable to confirm the triclopyricarb residues in wheat grain,straw and soil.

关 键 词：QUECHERS 超高效液相色谱-串联质谱 氯啶菌酯 小麦 土壤 

分 类 号：O657.63[理学—分析化学]