Targeted Multiresidue Method for the Analysis of Different Classes of Pesticides in Agro-Food Industrial Sludge by Liquid Chromatography Tandem Mass Spectrometry

Sludge generated after washing of fruits and vegetables during agro-food processes is a complex matrix and selective methods for the identification and quantification of pesticides’ residues are necessary in order to achieve a sustainable and effective management of the total sewage. The present wor...

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Main Authors: Niki C. Maragou, George Balayiannis, Evangelos Karanasios, Emilia Markellou, Konstantinos Liapis
Format: Article
Language:English
Published: MDPI AG 2021-11-01
Series:Molecules
Subjects:
Online Access:https://www.mdpi.com/1420-3049/26/22/6888
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author Niki C. Maragou
George Balayiannis
Evangelos Karanasios
Emilia Markellou
Konstantinos Liapis
author_facet Niki C. Maragou
George Balayiannis
Evangelos Karanasios
Emilia Markellou
Konstantinos Liapis
author_sort Niki C. Maragou
collection DOAJ
description Sludge generated after washing of fruits and vegetables during agro-food processes is a complex matrix and selective methods for the identification and quantification of pesticides’ residues are necessary in order to achieve a sustainable and effective management of the total sewage. The present work describes the development and validation of a reliable, simple and fast analytical method based on liquid chromatography-tandem mass spectrometry (LC-MS/MS) for the determination of 47 pesticides of different chemical classes, including organosphosphates, pyrethroids, neonicotinoids, triazoles and others, in sludge samples after QuEChERS sample preparation. The necessity of the individual steps of QuEChERS was investigated and the LC-ESI-MS/MS conditions were optimized to achieve maximum sensitivity of the target analytes. The method limits of detection (LODs) ranged between 0.0005 mg/kg (imidacloprid) and 0.05 mg/kg (beta cyfluthrin). The recoveries ranged between 71–120% and the repeatability of the method was ≤25% expressed as relative standard deviation. The method was applied to sludge samples generated after washing of fruits in an agro-fruit-packaging unit in Greece. The results showed the presence of 37 pesticides’ active substances with concentrations ranging from low ppbs, such as fludioxinil (5 μg/kg) up to low ppms such as beta cyfluthrin (3.5 mg/kg) and with their sum concentration reaching up to 19 mg/kg.
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spelling doaj.art-69b28c4c25c5429ab13483dd896b68b42023-11-23T00:35:13ZengMDPI AGMolecules1420-30492021-11-012622688810.3390/molecules26226888Targeted Multiresidue Method for the Analysis of Different Classes of Pesticides in Agro-Food Industrial Sludge by Liquid Chromatography Tandem Mass SpectrometryNiki C. Maragou0George Balayiannis1Evangelos Karanasios2Emilia Markellou3Konstantinos Liapis4Laboratory of Chemical Control of Pesticides, Scientific Directorate of Pesticides’ Control and Phytopharmacy, Benaki Phytopathological Institute, 14561 Athens, GreeceLaboratory of Chemical Control of Pesticides, Scientific Directorate of Pesticides’ Control and Phytopharmacy, Benaki Phytopathological Institute, 14561 Athens, GreeceLaboratory of Environmental Control of Pesticides, Scientific Directorate of Pesticides’ Control & Phytopharmacy, Benaki Phytopathological Institute, 14561 Athens, GreeceLaboratory of Mycology, Scientific Directorate of Phytopathology, Benaki Phytopathological Institute, 14561 Athens, GreeceLaboratory of Pesticide Residues, Scientific Directorate of Pesticides’ Control and Phytopharmacy, Benaki Phytopathological Institute, 14561 Athens, GreeceSludge generated after washing of fruits and vegetables during agro-food processes is a complex matrix and selective methods for the identification and quantification of pesticides’ residues are necessary in order to achieve a sustainable and effective management of the total sewage. The present work describes the development and validation of a reliable, simple and fast analytical method based on liquid chromatography-tandem mass spectrometry (LC-MS/MS) for the determination of 47 pesticides of different chemical classes, including organosphosphates, pyrethroids, neonicotinoids, triazoles and others, in sludge samples after QuEChERS sample preparation. The necessity of the individual steps of QuEChERS was investigated and the LC-ESI-MS/MS conditions were optimized to achieve maximum sensitivity of the target analytes. The method limits of detection (LODs) ranged between 0.0005 mg/kg (imidacloprid) and 0.05 mg/kg (beta cyfluthrin). The recoveries ranged between 71–120% and the repeatability of the method was ≤25% expressed as relative standard deviation. The method was applied to sludge samples generated after washing of fruits in an agro-fruit-packaging unit in Greece. The results showed the presence of 37 pesticides’ active substances with concentrations ranging from low ppbs, such as fludioxinil (5 μg/kg) up to low ppms such as beta cyfluthrin (3.5 mg/kg) and with their sum concentration reaching up to 19 mg/kg.https://www.mdpi.com/1420-3049/26/22/6888fungicidesinsecticidesagricultural productsmethod optimizationextractionenvironmentally friendly
spellingShingle Niki C. Maragou
George Balayiannis
Evangelos Karanasios
Emilia Markellou
Konstantinos Liapis
Targeted Multiresidue Method for the Analysis of Different Classes of Pesticides in Agro-Food Industrial Sludge by Liquid Chromatography Tandem Mass Spectrometry
Molecules
fungicides
insecticides
agricultural products
method optimization
extraction
environmentally friendly
title Targeted Multiresidue Method for the Analysis of Different Classes of Pesticides in Agro-Food Industrial Sludge by Liquid Chromatography Tandem Mass Spectrometry
title_full Targeted Multiresidue Method for the Analysis of Different Classes of Pesticides in Agro-Food Industrial Sludge by Liquid Chromatography Tandem Mass Spectrometry
title_fullStr Targeted Multiresidue Method for the Analysis of Different Classes of Pesticides in Agro-Food Industrial Sludge by Liquid Chromatography Tandem Mass Spectrometry
title_full_unstemmed Targeted Multiresidue Method for the Analysis of Different Classes of Pesticides in Agro-Food Industrial Sludge by Liquid Chromatography Tandem Mass Spectrometry
title_short Targeted Multiresidue Method for the Analysis of Different Classes of Pesticides in Agro-Food Industrial Sludge by Liquid Chromatography Tandem Mass Spectrometry
title_sort targeted multiresidue method for the analysis of different classes of pesticides in agro food industrial sludge by liquid chromatography tandem mass spectrometry
topic fungicides
insecticides
agricultural products
method optimization
extraction
environmentally friendly
url https://www.mdpi.com/1420-3049/26/22/6888
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