作　　者： (董亚蕾）; (刘文婧）; (曹进）; (王钢力）;

机构地区： 中国食品药品检定研究院,北京100050

出　　处： 《分析化学》 2017年第9期1397-1404,共8页

摘　　要： 建立了检测4种坚果(花生、杏仁、腰果、核桃)中38种农药残留的Qu ECh ERS-超高效液相色谱-串联质谱(UPLC-MS/MS)方法。样品均质后,用乙腈进行提取,经PSA和C_(18)净化后,采用Oasis PRi ME HLB固相萃取柱进一步净化,UPLC-MS/MS分析。对样品前处理和色谱方法进行了优化。在多重反应监测(MRM)模式下进行质谱分析,外标法定量。38种农药的检出限范围(S/N=3)为0.01~10μg/kg,定量限(S/N=10)为0.05~20μg/kg,线性关系良好(r>0.991)。4种坚果中农药的平均加标回收率为51.0%~126.0%,相对标准偏差均小于20%。此方法灵敏、准确、有效,可用于坚果类食品中多种农药残留的同时测定。 A multi-residue analysis method was developed for the determination of 38 kinds of pesticides in nuts（ almonds, peanuts, cashew nuts and walnuts） by Qu ECh ERS-ultra-high performance liquid chromatography-tandem mass spectrometry. The pesticide residues were extracted with acetonitrile. The extract was cleaned up with PSA,C18 and Oasis PRi ME HLB,and then analyzed by UPLC-MS/MS with multiple reaction monitoring（ MRM） mode. External standard method was employed to quantify. The limits of detection（ LODs,S/N = 3） of this method were between 0. 01 and 10 μg/kg,and the limits of quantitation（ LOQs,S/N=10） were between 0. 05-20 μg/kg. All of the tested pesticides showed good linear relationship（ r〉0. 991）. The practical samples were determined at three spiked levels and the average recoveries were between 51. 0% and 126. 0%. The RSDs were less than 20%. This method was simple,sensitive and accurate,and could be used for the routine analysis of pesticide residues in nuts.

关 键 词： 超高效液相色谱 串联质谱 农药残留 坚果