Selective and Sensitive Quantification of Acetochlor and S-Metolachlor in Maize and Soybean Plant Samples by Gas Chromatography-Tandem Mass Spectrometry

Herbicide residue analysis has gained importance worldwide, mainly for food quality control to minimize potentially adverse impacts on human health. A Gas chromatography-tandem mass spectrometry (GC-MS) method for quantitative analysis of acetochlor and s-metolachlor in maize and soybean straw has b...

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Main Authors: Irina Gabriela Cara, Denis Topa, Lucian Raus, Anca Elena Calistru, Feodor Filipov, Gerard Jitareanu
Format: Article
Language:English
Published: MDPI AG 2021-03-01
Series:Agriculture
Subjects:
Online Access:https://www.mdpi.com/2077-0472/11/4/283
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author Irina Gabriela Cara
Denis Topa
Lucian Raus
Anca Elena Calistru
Feodor Filipov
Gerard Jitareanu
author_facet Irina Gabriela Cara
Denis Topa
Lucian Raus
Anca Elena Calistru
Feodor Filipov
Gerard Jitareanu
author_sort Irina Gabriela Cara
collection DOAJ
description Herbicide residue analysis has gained importance worldwide, mainly for food quality control to minimize potentially adverse impacts on human health. A Gas chromatography-tandem mass spectrometry (GC-MS) method for quantitative analysis of acetochlor and s-metolachlor in maize and soybean straw has been developed, validated and applied to analyze the residues of anilide herbicides. Straw material was dried, homogenized and extracted with a mixture of n-hexane and acetone by an accelerated solvent extraction method. Chromatographic separation of the target analytes was performed on an Agilent 7832 GC equipped with a mass spectrometer detector, a split-splitless injector and an HP-5 MS (5% phenylmethyl siloxane) capillary column (30 m × 0.25 mm × 0.25 µm). Under these parameters, the limit of detection (LOD) values were 0.2 ng g<sup>−1</sup> for acetochlor and 0.07 ng g<sup>−1</sup> for s-metolachlor, with average recoveries between 86% and 119.7%. The method was validated for acetochlor and s-metolachlor in maize and soybean straw at 0.5 and 0.01 mg kg <sup>−1</sup>. Furthermore, the final residues of the two herbicides in maize and soybean straw were below the maximum residue limit (MRL) at harvest time. The proposed method is suitable for routine analysis.
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spelling doaj.art-f5e7f8ef9de040309b535e775ddc1e072023-11-21T12:01:24ZengMDPI AGAgriculture2077-04722021-03-0111428310.3390/agriculture11040283Selective and Sensitive Quantification of Acetochlor and S-Metolachlor in Maize and Soybean Plant Samples by Gas Chromatography-Tandem Mass SpectrometryIrina Gabriela Cara0Denis Topa1Lucian Raus2Anca Elena Calistru3Feodor Filipov4Gerard Jitareanu5Research Institute for Agriculture and Environment, “Ion Ionescu de la Brad” University of Agricultural Sciences and Veterinary Medicine, 700490 Iasi, RomaniaDepartment of Pedotechnics, Faculty of Agriculture, “Ion Ionescu de la Brad” University of Agricultural Sciences and Veterinary Medicine, 700490 Iasi, RomaniaDepartment of Pedotechnics, Faculty of Agriculture, “Ion Ionescu de la Brad” University of Agricultural Sciences and Veterinary Medicine, 700490 Iasi, RomaniaDepartment of Pedotechnics, Faculty of Agriculture, “Ion Ionescu de la Brad” University of Agricultural Sciences and Veterinary Medicine, 700490 Iasi, RomaniaDepartment of Pedotechnics, Faculty of Agriculture, “Ion Ionescu de la Brad” University of Agricultural Sciences and Veterinary Medicine, 700490 Iasi, RomaniaDepartment of Pedotechnics, Faculty of Agriculture, “Ion Ionescu de la Brad” University of Agricultural Sciences and Veterinary Medicine, 700490 Iasi, RomaniaHerbicide residue analysis has gained importance worldwide, mainly for food quality control to minimize potentially adverse impacts on human health. A Gas chromatography-tandem mass spectrometry (GC-MS) method for quantitative analysis of acetochlor and s-metolachlor in maize and soybean straw has been developed, validated and applied to analyze the residues of anilide herbicides. Straw material was dried, homogenized and extracted with a mixture of n-hexane and acetone by an accelerated solvent extraction method. Chromatographic separation of the target analytes was performed on an Agilent 7832 GC equipped with a mass spectrometer detector, a split-splitless injector and an HP-5 MS (5% phenylmethyl siloxane) capillary column (30 m × 0.25 mm × 0.25 µm). Under these parameters, the limit of detection (LOD) values were 0.2 ng g<sup>−1</sup> for acetochlor and 0.07 ng g<sup>−1</sup> for s-metolachlor, with average recoveries between 86% and 119.7%. The method was validated for acetochlor and s-metolachlor in maize and soybean straw at 0.5 and 0.01 mg kg <sup>−1</sup>. Furthermore, the final residues of the two herbicides in maize and soybean straw were below the maximum residue limit (MRL) at harvest time. The proposed method is suitable for routine analysis.https://www.mdpi.com/2077-0472/11/4/283acetochlors-metolachlorresiduesplant samplesGC-MS
spellingShingle Irina Gabriela Cara
Denis Topa
Lucian Raus
Anca Elena Calistru
Feodor Filipov
Gerard Jitareanu
Selective and Sensitive Quantification of Acetochlor and S-Metolachlor in Maize and Soybean Plant Samples by Gas Chromatography-Tandem Mass Spectrometry
Agriculture
acetochlor
s-metolachlor
residues
plant samples
GC-MS
title Selective and Sensitive Quantification of Acetochlor and S-Metolachlor in Maize and Soybean Plant Samples by Gas Chromatography-Tandem Mass Spectrometry
title_full Selective and Sensitive Quantification of Acetochlor and S-Metolachlor in Maize and Soybean Plant Samples by Gas Chromatography-Tandem Mass Spectrometry
title_fullStr Selective and Sensitive Quantification of Acetochlor and S-Metolachlor in Maize and Soybean Plant Samples by Gas Chromatography-Tandem Mass Spectrometry
title_full_unstemmed Selective and Sensitive Quantification of Acetochlor and S-Metolachlor in Maize and Soybean Plant Samples by Gas Chromatography-Tandem Mass Spectrometry
title_short Selective and Sensitive Quantification of Acetochlor and S-Metolachlor in Maize and Soybean Plant Samples by Gas Chromatography-Tandem Mass Spectrometry
title_sort selective and sensitive quantification of acetochlor and s metolachlor in maize and soybean plant samples by gas chromatography tandem mass spectrometry
topic acetochlor
s-metolachlor
residues
plant samples
GC-MS
url https://www.mdpi.com/2077-0472/11/4/283
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