A simple; efficient and environmentally friendly method for the extraction of pesticides from onion by matrix solid-phase dispersion with liquid chromatography-tandem mass spectrometric detection

被引:58
作者
Rodrigues, Sherol Acosta [1 ]
Caldas, Sergiane Souza [1 ]
Primel, Ednei Gilberto [1 ]
机构
[1] Univ Fed Rio Grande, Postgrad Program Technol & Environm Chem, Escola Quim & Alimentos, BR-96201900 Rio Grande, RS, Brazil
关键词
Sorbent; Matrix solid-phase dispersion; Onion; Pesticide; Liquid chromatography-tandem mass spectrometry; SUPERCRITICAL-FLUID EXTRACTION; SAMPLE PREPARATION TECHNIQUES; GAS-CHROMATOGRAPHY; RESIDUE ANALYSIS; MULTIRESIDUE DETERMINATION; NEW-GENERATION; OLIVE OIL; FRUITS; ANTIOXIDANT; FUNGICIDE;
D O I
10.1016/j.aca.2010.08.026
中图分类号
O65 [分析化学];
学科分类号
070302 ; 081704 ;
摘要
An evaluation of the extraction of pesticides from onion by matrix solid-phase dispersion (MSPD) with the determination by liquid chromatography tandem mass spectrometry using electrospray as the ionization source (LC-ESI-MS/MS) was carried out. The performance of different sorbents, including reused C18 bonded silica, was evaluated. Different parameters affecting the extraction efficiency were evaluated, such as the type and amount of sorbent. the time of interaction after the fortification step, the time of sample dispersion and the elution solvent. The matrix effect regarding the recovery of the pesticides by MSPD was also investigated. The best results were obtained using 0.5 g of sample, 1.0 g reused C18, interaction time of 1 h, dispersion time of 5 min, and acetonitrile as the elution solvent. The method was validated by the fortification of the onion sample, free of pesticides, at different concentration levels (0.01, 0.1 and 1.0 mg kg(-1)). Average recoveries ranged from 78.3 to 120.4% and relative standard deviation below 20% was obtained. Detection and quantification limits ranged from 0.003 to 0.03 mg kg(-1) and from 0.01 to 0.1 mg kg(-1), respectively. (C) 2010 Elsevier B.V. All rights reserved.
引用
收藏
页码:82 / 89
页数:8
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