Determination of Haloxyfop-Methyl, Linuron, and Procymidone Pesticides in Carrot Using SLE-LTP Extraction and GC-MS

Abstract

This study aimed to optimize and validate an analytical method for extraction, detection, and quantification of haloxyfop-methyl, procymidone, and linuron pesticides in carrot samples using solid-liquid extraction methods and low temperature partition (SLE-LTP), accompanied by gas chromatography coupled to mass spectrometry (GC-MS). For SLE-LTP technical optimization, we utilized a complete factorial planning, which had as its variables, agitation time, freezing time, and the correct sample mass/extracting solution volume ratio. The organic extract obtained was analyzed by GC-MS. To test the performance of this procedure, the method was validated and applied to the monitoring of pesticide residues in 20 samples of carrot produced in Alto Paranaíba, Minas Gerais, Brazil. The proposed method showed linearity between 0.5 and 3.5 mg·kg −1 with correlation coefficients greater than 0.99. The quantification limits were 0.48 mg· kg −1 for haloxyfop-methyl, 0.69 mg·kg −1 for linuron, and 0.65 mg·kg −1 for procymidone, values below the maximum residue limit provided by international legislation of 1.0 mg· kg −1 for linuron and procymidone. The use of haloxyfopmethyl is not approved in the cultivation of carrot. The recovery percentages were between 90 and 110 %, with a coefficient of variation of less than 12 %. Ten percent of the carrot samples monitored showed residues of linuron and procymidone in concentrations exceeding those permitted by Brazilian law.

Avaliação da ESL-PBT na determinação de carbaril em amostras de abacaxi pérola (ananás comosus) comercializadas no município de Itumbiara

“…Em contrapartida, outro método que foi desenvolvido e que tem sido utilizado com sucesso para determinação de agrotóxicos em alimentos e demais amostras por cromatografia é a extração sólido-líquido com partição em baixa temperatura (ESL/PBT) [20][21]. O método permite o desempenho simultâneo pela extração de agrotóxicos e limpeza dos extratos e inúmeros estudos também já foram realizados, sendo aplicado em amostras frutíferas e de origem vegetal, como na batata [22], cenoura [23], abobrinha [24], alface [25], alho [26], milho [27], tomates [28], cajá-manga [29], pimentão [30] e aplicado em amostras de solos [31][32][33]. O método é simples, eficiente, oferece praticidade, baixo consumo de solvente orgânico e amostra, número reduzido de etapas e confiabilidade com porcentagens de recuperação elevadas e boa repetitividade [34].…”

Development of a Methodology for the Determination of Pesticide Residues in Cajá-Manga Pulp (Spondias dulcisL.) Using Solid-Liquid Extraction with Low-Temperature Partitioning

“…e solid-liquid extraction with low-temperature partitioning (SLE-LTP) was used in this study because it is an efficient method in the extraction of pesticide residues from different samples [19][20][21][22][23][34][35][36][37] and, mainly, because it is an easy application method involving few steps and low consumption of solvents and sorbents compared to other extraction methods. e SLE-LTP was optimized for the extraction of pesticide residues from the cajá-manga pulp to obtain maximum recovery of the analytes.…”

“…is decantation appears to increase gradually with increasing freezing time, leading to the pesticide adsorptions on the frozen phase surface and reducing their recoveries. In the literature, freezing times greater than 3 h are recorded for efficient extraction of pesticides from other matrices [19,22,23,35]. As the composition of the cajámanga pulp is approximately 70% water and low content of liposoluble components, the extraction of residues of the compounds studied occurred more quickly [5].…”

Development of a dispersive liquid-liquid microextraction technique for the analysis of aryloxyphenoxy-propionate herbicides in soy-based foods

“…The widespread use of those compounds contributes to their presence in ground water, soil and other environmental matrices [4,5]. Recently there have been a few reported studies on the determination of some AOPPs in water [6][7][8][9][10][11], soils [12,13], crops [12,14], fruits and vegetables [9,15]. However, any analytical methodology to determine AOPPs in processed foods, specifically in crops-derived ones such as soy-sauce or soy milk, have been developed.…”