Albero Beatriz, Sánchez-Brunete Consuelo, Tadeo José L
Departamento de Medio Ambiente, INIA, Carretera de la Coruña Km 7, 28040 Madrid, Spain.
J Agric Food Chem. 2003 Nov 19;51(24):6915-21. doi: 10.1021/jf030414m.
A rapid multiresidue method was developed for the determination of nine organophosphorus pesticides in fruit juices. The analytical procedure is based on the matrix solid-phase dispersion (MSPD) of juice samples on Florisil in small glass columns and subsequent extraction with ethyl acetate assisted by sonication. Residue levels were determined by gas chromatography with nitrogen-phosphorus detection. Spiked blank samples were used as standards to counteract the matrix effect observed in the chromatographic determination. The NPD response for all pesticides was linear in the concentration range studied with determination coefficients >0.999. Average recoveries obtained for all of the pesticides in the different juices and fortification levels were >70% with relative standard deviations of <11%. The detection limits ranged from 0.1 to 0.6 microg/kg. The identity of the pesticides was confirmed by gas chromatography with mass spectrometric detection using selected ion monitoring. The proposed MSPD method was applied to determine pesticide residue levels in fruit juices sold in Spanish supermarkets. At least one pesticide was found in most of the samples, although the levels detected were very low, far from the maximum residue levels established for raw fruit.
建立了一种快速多残留方法，用于测定果汁中的9种有机磷农药。分析程序基于果汁样品在小玻璃柱中的弗罗里硅土上的基质固相分散（MSPD），随后通过超声辅助用乙酸乙酯萃取。残留水平通过带有氮磷检测的气相色谱法测定。加标空白样品用作标准品，以抵消色谱测定中观察到的基质效应。在所研究的浓度范围内，所有农药的NPD响应呈线性，测定系数>0.999。不同果汁和强化水平下所有农药的平均回收率>70%，相对标准偏差<11%。检测限范围为0.1至0.6微克/千克。通过使用选择离子监测的带有质谱检测的气相色谱法确认农药的身份。所提出的MSPD方法应用于测定西班牙超市销售的果汁中的农药残留水平。在大多数样品中至少发现了一种农药，尽管检测到的水平非常低，远低于为生鲜水果设定的最大残留水平。
