Comparison of different extraction methods for the simultaneous determination of pesticide residues in kiwi fruit using gas chromatography–mass spectrometry

Abstract

The methods of simultaneous extraction of iprodione, chlorpyrifos-methyl, EPN and endosulfan (with its metabolites) from kiwi fruit using accelerated solvent extraction (ASE), supercritical fluid extraction (SFE), and liquid-liquid extraction (LLE) were tested and compared in terms of their of limits of detection and quantification, as well as the highest pesticide recoveries with the lowest residues in the final extracts. The analysis was performed using gas chromatography-mass spectrometry in the selected ion monitoring mode. The proposed methods featured good sensitivity, pesticide quantification limits were low enough, and the precision (expressed as relative standard deviations) ranged from 0.56 to 7.17%. The recoveries obtained from ASE, SFE and LLE were 77.5-120, 71.9-109.1 and 75.6-127.1%, respectively. The proposed methods were successfully applied for the monitoring of the selected pesticide residues in kiwi fruit samples collected from Jollanamdo area, Republic of Korea. Iprodione was detected at a level lower than the maximum residue limit (MRL) established by the Korea Food and Drug Administration (5 ppm), while EPN was detected at a level higher than the Korea Food and Drug Administration MRL (0.1 ppm) in the real samples. The proposed sample preparations led to a higher preconcentration of the pesticide fraction, and allowed the sensitive and selective determination of pesticides with varied physicochemical properties in kiwi fruit.

Técnicas de análise de resíduos de agrotóxicos em alimentos de origem vegetal: uma revisão

“…É uma técnica de extração rápida e que reduz consideravelmente a quantidade de solvente, e por meio da otimização de alguns parâmetros como temperatura, pressão e polaridade do solvente é possível obter boas recuperações. A desvantagem incide no fato de diferentes propriedades físico-químicas dos analitos dificultarem o emprego em análises multirresíduo [18,[21][22][23] .…”

Extração em Fase Sólida Dispersiva na determinação de resíduos e contaminantes em alimentos

“…É uma técnica de extração rápida e que reduz consideravelmente a quantidade de solvente [23] . Com a otimização de alguns parâme-tros como temperatura, pressão e polaridade do solvente é possível obterem boas recuperações com a PLE [24] , no entanto as diferentes propriedades físico-químicas dos analitos dificultam o emprego em análises multirresíduo. A Extração Assistida por Micro-ondas (Microwave-Assisted Extraction, MAE) foi utilizada pela primeira vez para extração de compostos orgânicos por Ganzler et al [25] , no entanto se tornou mais popular recentemente.…”

Modern Extraction Techniques for Pesticide Residues Determination in Plant and Soil Samples

“…Thus, Di Muccio et al (2006) developed ASE method for neonicotinoids determination in apricot, peach, pear, celery and zucchini. Richter et al (2001) developed ASE for OPPs determination in carrot, Wennrich et al (2001) for OCPs in strawberry, apple, lettuce, tomato and kohlrabi, while Cho et al (2008) tested ASE for determination of iprodione, chlorpyrifos-methyl and endosulfan in kiwi. In 2007, Barriada-Pereira et al described it as a satisfactory method for determining 21 OCPs in lettuce, tomato, spinach, potato, tomato and bean, and in the same year Carabias-Martínez et al (2007) used ASE to determine triazines in potato, carrot, lettuce, bean, zucchini and orange.…”