Citation: DONG Ya-Lei, LIU Wen-Jing, CAO Jin, WANG Gang-Li. Determination of 38 Kinds of Pesticide Residues in Nuts by QuEChERS-Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry. Chinese Journal of Analytical Chemistry, 2017, 45(9): 1397-1404. doi: 10.11895/j.issn.0253-3820.160885 [复制]
Determination of 38 Kinds of Pesticide Residues in Nuts by QuEChERS-Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry
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QuEChERS-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C18净化后，采用Oasis PRiME 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0.01~10 μg/kg，定量限（S/N=10）为0.05~20 μg/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 QuEChERS-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 PRiME 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.
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