Albero Beatriz, Sánchez-Brunete Consuelo, Tadeo José L
Departamento de Medio Ambiente, INIA, Ctra. de la Coruña Km. 7, 28040 Madrid, Spain.
Talanta. 2005 May 15;66(4):917-24. doi: 10.1016/j.talanta.2004.12.046. Epub 2005 Jan 20.
A multiresidue method based on solid-phase extraction was developed for the simultaneous determination of 50 pesticides in commercial juices. The extraction procedure was carried out in C(18) columns preconditioned with acetonitrile and water. The subsequent elution of pesticides was performed with a mixture of hexane-ethyl acetate (1:1, v/v) prior to the determination by gas chromatography with electron impact mass spectrometric detection in the selected ion monitoring mode (GC-MS-SIM), using one target and two qualifier ions. Standards were prepared spiking blank juice samples to counteract the observed matrix effect. Average recoveries for all the pesticides studied were higher than 91% with relative standard deviations lower than 9% in the concentration range of 0.02-0.1mug/mL and the detection limits achieved ranged from 0.1 to 4.6mug/L. The proposed method was applied to the analysis of these compounds in commercial juices and diazinon, ethion and procymidone were the pesticides encountered, although the levels found were very low.
建立了一种基于固相萃取的多残留方法，用于同时测定市售果汁中的50种农药。萃取过程在先用乙腈和水预处理的C(18)柱上进行。在通过气相色谱-电子轰击质谱检测（GC-MS-SIM）在选择离子监测模式下进行测定之前，先用己烷-乙酸乙酯（1:1，v/v）混合物洗脱农药，使用一个目标离子和两个定性离子。通过向空白果汁样品中添加标准品来制备标准品，以抵消观察到的基质效应。在所研究的所有农药中，在0.02-0.1μg/mL的浓度范围内，平均回收率高于91%，相对标准偏差低于9%，检测限为0.1至4.6μg/L。该方法应用于市售果汁中这些化合物的分析，虽然发现的水平很低，但仍检测到了二嗪农、乙硫磷和腐霉利。
