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

Niki C Maragou,George Balayiannis,Evangelos Karanasios,Emilia Markellou,Konstantinos Liapis

doi:10.3390/molecules26226888

Niki C Maragou, George Balayiannis + Show 3 more

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https://doi.org/10.3390/molecules26226888

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Abstract

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.

Highlights

Agro-food processes usually concern washing of fruits and vegetables before packaging and distribution to the market
Matrix solid-phase dispersion (MSPD) has been applied for the determination of fifteen pesticides belonging to the organophosphate, triazine, organochlorine, triazole, pyrethroid, carbamate and other chemical groups in drinking water treatment sludge followed by GC-MS analysis [3]
The aim of the present work was the development of a QuEChERS based sample preparation followed by LC-electrospray ionization interface (ESI)-triple quadrupole MS/MS method after a stepwise optimization, which allows the simultaneous determination of a large number of pesticides that belong to different chemical classes in sludge at the low ng/g level

Summary

Introduction

Agro-food processes usually concern washing of fruits and vegetables before packaging and distribution to the market. Sludge is a complex and difficult matrix to analyze, and suitable and reliable methods are required for the determination of contaminants present at low levels such as pesticides. Complex matrices such as sludge usually involve labor-intensive extraction and cleanup procedures before the chromatographic analysis [1]. Matrix solid-phase dispersion (MSPD) has been applied for the determination of fifteen pesticides belonging to the organophosphate, triazine, organochlorine, triazole, pyrethroid, carbamate and other chemical groups in drinking water treatment sludge followed by GC-MS analysis [3]. Comparison between PLE and QuEChERS showed that the second was superior for samples of sediment, soil and sludge [5]

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