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占绣萍, 陈建波, 马琳, 等. 超高效液相色谱-质谱联用法测定蔬菜中多杀霉素等4种农药残留[J]. 分析测试学报, 2016,35(4):476-481.
Simultaneous Determination of Four Pesticides Residues in Vegetables by Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry[J]. 2016,35(4):476-481.
采用固相萃取/超高效液相色谱-串联质谱(SPE/UPLC-MS/MS)建立了多种蔬菜中4种农药残留量的分析方法,并对净化方法、色谱及质谱条件进行优化。蔬菜样品经乙腈提取、提取液经盐析后,取上清液经PC/NH2(或NH2)固相萃取小柱净化,浓缩后,用甲醇定容并过膜,采用超高效液相色谱-串联质谱多反应监测(MRM)正离子模式进行外标法定量测定。结果表明,4种农药在5~500 μg/L范围内线性关系良好(r≥0.999 2),在8种蔬菜中的检出限和定量下限分别为0.033~0.167 μg/kg和0.10~0.50 μg/kg 。在10,50,250 μg/kg 3个浓度加标水平下,4种农药的回收率为70.9%~123.4%,相对标准偏差(RSD)小于15%。方法准确、灵敏、简单、快速,适用于多种蔬菜中多杀霉素等4种农药残留的同时测定。
A method was developed for the determination of four pesticides residues in a variety of vegetables using solid phase extraction(SPE) and ultra performance liquid chromatography-triple quadrupole-mass spectrometry(UPLC-MS/MS).The purification methods(solid phase extraction column,QuEChERS method,elution solvent,elution volume),chromatographic conditions(mobile phase type,flow rate and column temperature) and mass spectrometric parameters(fragment,delta EMV) were optimized.The pesticides samples were extracted with acetonitrile,and then cleaned up on a Carbon/NH2(or NH2) SPE column.The eluting solution was evaporated and made up to a definite volumn with methanol,finally analyzed by reversed phase ultra performance liquid chromatography under multiple reaction monitoring(MRM) of positive ion mode with the external standard method.The calibration curves of four pesticides showed good linearities in the range of 5-500 μg/L with correlation coefficients not less than 0.999 2.The limits of detection(LOD) were in the range of 0.033-0.167 μg/kg and the limits of quantitation(LOQ) were in the range of 0.10-0.50 μg/kg for 4 pesticides spiked in vegetable.The recoveries of 4 pesticides in vegetable sample spiked with three concentration levels of 10,50,250 μg/kg ranged from 70.9% to 123.4% with RSDs less than 15%.The established method was accurate,sensitive and simple,and was suitable for the simultaneous analysis of various pesticides residues.
超高效液相色谱-质谱联用固相萃取农药残留蔬菜
ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)solid phase extraction(SPE)pesticide residuevegetable
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