Development of a Microwave-Assisted Extraction Protocol for the Simultaneous Determination of Mycotoxins and Pesticide Residues in Apples by LC-MS/MS

The possible presence of contaminants, pesticide residues and mycotoxins, in agricultural commodities is a critical issue for food safety, causing great concern. In this work, a simple and rapid analytical method employing liquid chromatography–tandem mass spectrometry (LC-MS/MS) was developed for t...

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Autores principales: Natasa P. Kalogiouri, Emmanouil-Nikolaos Papadakis, Maria G. Maggalou, George S. Karaoglanidis, Victoria F. Samanidou, Urania Menkissoglu-Spiroudi
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Publicado: MDPI AG 2021
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spelling oai:doaj.org-article:14a23661e3654f0786bc275e0007f25a2021-11-25T16:41:17ZDevelopment of a Microwave-Assisted Extraction Protocol for the Simultaneous Determination of Mycotoxins and Pesticide Residues in Apples by LC-MS/MS10.3390/app1122109312076-3417https://doaj.org/article/14a23661e3654f0786bc275e0007f25a2021-11-01T00:00:00Zhttps://www.mdpi.com/2076-3417/11/22/10931https://doaj.org/toc/2076-3417The possible presence of contaminants, pesticide residues and mycotoxins, in agricultural commodities is a critical issue for food safety, causing great concern. In this work, a simple and rapid analytical method employing liquid chromatography–tandem mass spectrometry (LC-MS/MS) was developed for the simultaneous determination of pesticide residues and mycotoxins in apples. Microwave-assisted extraction (MAE) was used for sample preparation. The MAE protocol was optimized after evaluating the effects of the following extraction parameters: (a) extraction solvent, (b) acidic environment, (c) temperature, and (d) extraction time. The multiresidue MAE-LC-MS/MS method was validated for linearity, accuracy (bias and precision), limits of detection (LODs), limits of quantification (LOQs), and matrix effect. The validation of the method was carried out according to the SANTE/12682/2019 document. The method demonstrated good linearity with R<sup>2</sup> ≥ 0.99, acceptable accuracy in the recovery rate range 70–116%, acceptable interassay precision with RSD% ≤ 20, and low LODs and LOQs in the ranges 0.005–0.015 μg/g and 0.01–0.03 μg/g, respectively. Matrix effects were observed only for the 25% of the analytes. The performance of the MAE-LC-MS/MS method was compared to that of the QuEChERS sample preparation method, and the MAE-LC-MS/MS method proved to be rapid and effective.Natasa P. KalogiouriEmmanouil-Nikolaos PapadakisMaria G. MaggalouGeorge S. KaraoglanidisVictoria F. SamanidouUrania Menkissoglu-SpiroudiMDPI AGarticlemycotoxinspesticidesmicrowave-assisted extractionLC-MS/MSTechnologyTEngineering (General). Civil engineering (General)TA1-2040Biology (General)QH301-705.5PhysicsQC1-999ChemistryQD1-999ENApplied Sciences, Vol 11, Iss 10931, p 10931 (2021)
institution DOAJ
collection DOAJ
language EN
topic mycotoxins
pesticides
microwave-assisted extraction
LC-MS/MS
Technology
T
Engineering (General). Civil engineering (General)
TA1-2040
Biology (General)
QH301-705.5
Physics
QC1-999
Chemistry
QD1-999
spellingShingle mycotoxins
pesticides
microwave-assisted extraction
LC-MS/MS
Technology
T
Engineering (General). Civil engineering (General)
TA1-2040
Biology (General)
QH301-705.5
Physics
QC1-999
Chemistry
QD1-999
Natasa P. Kalogiouri
Emmanouil-Nikolaos Papadakis
Maria G. Maggalou
George S. Karaoglanidis
Victoria F. Samanidou
Urania Menkissoglu-Spiroudi
Development of a Microwave-Assisted Extraction Protocol for the Simultaneous Determination of Mycotoxins and Pesticide Residues in Apples by LC-MS/MS
description The possible presence of contaminants, pesticide residues and mycotoxins, in agricultural commodities is a critical issue for food safety, causing great concern. In this work, a simple and rapid analytical method employing liquid chromatography–tandem mass spectrometry (LC-MS/MS) was developed for the simultaneous determination of pesticide residues and mycotoxins in apples. Microwave-assisted extraction (MAE) was used for sample preparation. The MAE protocol was optimized after evaluating the effects of the following extraction parameters: (a) extraction solvent, (b) acidic environment, (c) temperature, and (d) extraction time. The multiresidue MAE-LC-MS/MS method was validated for linearity, accuracy (bias and precision), limits of detection (LODs), limits of quantification (LOQs), and matrix effect. The validation of the method was carried out according to the SANTE/12682/2019 document. The method demonstrated good linearity with R<sup>2</sup> ≥ 0.99, acceptable accuracy in the recovery rate range 70–116%, acceptable interassay precision with RSD% ≤ 20, and low LODs and LOQs in the ranges 0.005–0.015 μg/g and 0.01–0.03 μg/g, respectively. Matrix effects were observed only for the 25% of the analytes. The performance of the MAE-LC-MS/MS method was compared to that of the QuEChERS sample preparation method, and the MAE-LC-MS/MS method proved to be rapid and effective.
format article
author Natasa P. Kalogiouri
Emmanouil-Nikolaos Papadakis
Maria G. Maggalou
George S. Karaoglanidis
Victoria F. Samanidou
Urania Menkissoglu-Spiroudi
author_facet Natasa P. Kalogiouri
Emmanouil-Nikolaos Papadakis
Maria G. Maggalou
George S. Karaoglanidis
Victoria F. Samanidou
Urania Menkissoglu-Spiroudi
author_sort Natasa P. Kalogiouri
title Development of a Microwave-Assisted Extraction Protocol for the Simultaneous Determination of Mycotoxins and Pesticide Residues in Apples by LC-MS/MS
title_short Development of a Microwave-Assisted Extraction Protocol for the Simultaneous Determination of Mycotoxins and Pesticide Residues in Apples by LC-MS/MS
title_full Development of a Microwave-Assisted Extraction Protocol for the Simultaneous Determination of Mycotoxins and Pesticide Residues in Apples by LC-MS/MS
title_fullStr Development of a Microwave-Assisted Extraction Protocol for the Simultaneous Determination of Mycotoxins and Pesticide Residues in Apples by LC-MS/MS
title_full_unstemmed Development of a Microwave-Assisted Extraction Protocol for the Simultaneous Determination of Mycotoxins and Pesticide Residues in Apples by LC-MS/MS
title_sort development of a microwave-assisted extraction protocol for the simultaneous determination of mycotoxins and pesticide residues in apples by lc-ms/ms
publisher MDPI AG
publishDate 2021
url https://doaj.org/article/14a23661e3654f0786bc275e0007f25a
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