Abstract

A sensitive LC–ESI-MS/MS method was developed for the determination of 165 pesticides in 50 citrus fruit samples collected in Sicily. Moreover, an evaluation of pesticides levels in the citrus layers (peel, albedo, and pulp) was carried out. The method presented acceptable trueness, precision, and linearity with LOQ of 5 μg/kg. The results obtained showed a high frequency of fungicides class pesticides in all the citrus samples examined (>95%) with the highest concentrations in the peel (4468 µg/Kg). A significant difference of concentrations was found between the layers of the citrus fruits analysed (p < 0.05). In particular, the peel and albedo present higher pesticides significantly higher than the pulp. Our findings confirming the widespread use of these substances in citrus cultivation and suggesting the importance of pesticides analysis in all the citrus fruit layers separately, considering the different interactions between the physicochemical characteristics of the matrices and the pesticides.

Highlights

  • Citrus fruits represent an important source of nutrition and health value since ancient time (Cicero et al 2015; Salvo et al 2016)

  • The LOQs obtained were up to 10 times lower than the Maximum Residue Levels (MRLs) established by the EU legislations, suggesting that the proposed method is favorable for the analysis of pesticides in food of plant origin (Vinale et al 2016; Celano et al 2018)

  • Imazalil (l-[2-(2.4-dichlorophenyl)-2-(2-propenyloxy)ethyl]-lHimidazole) was the most detected pesticide in orange samples with a frequency of 83.3% confirming the wide use of this compound in citrus fruits cultivation due to its high activity against Penicillium spp. (Lafuente & Tadeo 1985)

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Summary

Introduction

Citrus fruits represent an important source of nutrition and health value since ancient time (Cicero et al 2015; Salvo et al 2016). Legal requirements of many countries are increasing, making it necessary to determine fungicide residues at very low levels. Despite the high number of works on the presence of pesticides in citrus fruits (Lafuente and Tadeo 1985; Ortelli et al 2005; Kanetis et al 2007; Phetkul et al 2014), further works are needed on the pesticides distribution from the pulp to the peel. The aim of the present work was to develop and validate a LC- MS/MS method for the simultaneous determination of 165 pesticides in citrus fruits collected in Sicily (Southern Italy) and investigate the pesticides distribution in the different layers (peel, albedo, and pulp)

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