Experimental Design and Multiple Response Optimization for the Extraction and Quantitation of Thirty-Four Priority Organic Micropollutants in Tomatoes through the QuEChERS Approach

The chemical contamination in fruit and vegetables represents a challenging analytical issue, with tomatoes deserving to be investigated as they are fundamental components of the Mediterranean diet. Polychlorinated biphenyls (PCBs), polycyclic aromatic hydrocarbons (PAHs) and nitro-PAHs contaminatio...

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Main Authors: Luca Rivoira, Massimo Del Bubba, Giasmin Cecconi, Michele Castiglioni, Valentina Testa, Mattia Isola, Maria Concetta Bruzzoniti
Format: Article
Language:English
Published: MDPI AG 2023-03-01
Series:Separations
Subjects:
Online Access:https://www.mdpi.com/2297-8739/10/3/174
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author Luca Rivoira
Massimo Del Bubba
Giasmin Cecconi
Michele Castiglioni
Valentina Testa
Mattia Isola
Maria Concetta Bruzzoniti
author_facet Luca Rivoira
Massimo Del Bubba
Giasmin Cecconi
Michele Castiglioni
Valentina Testa
Mattia Isola
Maria Concetta Bruzzoniti
author_sort Luca Rivoira
collection DOAJ
description The chemical contamination in fruit and vegetables represents a challenging analytical issue, with tomatoes deserving to be investigated as they are fundamental components of the Mediterranean diet. Polychlorinated biphenyls (PCBs), polycyclic aromatic hydrocarbons (PAHs) and nitro-PAHs contamination is of serious concern, due to particulate deposition and to uptake from contaminated soils and water. However, time-consuming, non-simultaneous and/or non-eco-friendly extraction procedures are typically used to investigate organic contamination in tomatoes, with nitro-PAHs that have not yet been studied. Based on these premises, this work reports the development of a QuEChERS-based approach, coupled with gas chromatography/mass spectrometry, for the simultaneous determination of 16 PAHs, 14 PCBs and 4 nitro-PAHs in three tomato cultivars. The effect of dichloromethane, cyclohexane and acetone, as well as of four clean-up phases were studied through the advanced combination of full factorial experimental design and multiple response optimization approaches. The final protocol, based on cyclohexane extraction followed by a double purification step with primary secondary amine and octadecyl silica and a sulfuric acid oxidation, led to 60–120% recoveries (RSD% < 15%). Good repeatability (inter-day precision <15%) and negligible matrix effect (<16%) were confirmed and the protocol was applied to the analysis of real tomato samples purchased in a local market.
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spelling doaj.art-be767b3e879e4e4b82532e4ddc11db032023-11-17T13:50:04ZengMDPI AGSeparations2297-87392023-03-0110317410.3390/separations10030174Experimental Design and Multiple Response Optimization for the Extraction and Quantitation of Thirty-Four Priority Organic Micropollutants in Tomatoes through the QuEChERS ApproachLuca Rivoira0Massimo Del Bubba1Giasmin Cecconi2Michele Castiglioni3Valentina Testa4Mattia Isola5Maria Concetta Bruzzoniti6Department of Chemistry, Università degli Studi di Torino, Via Pietro Giuria 7, 10125 Torino, ItalyDepartment of Chemistry “Ugo Schiff”, Università degli Studi di Firenze, Via della Lastruccia 13, 50019 Sesto Fiorentino, ItalyDepartment of Chemistry, Università degli Studi di Torino, Via Pietro Giuria 7, 10125 Torino, ItalyDepartment of Chemistry, Università degli Studi di Torino, Via Pietro Giuria 7, 10125 Torino, ItalyDepartment of Chemistry, Università degli Studi di Torino, Via Pietro Giuria 7, 10125 Torino, ItalyDepartment of Chemistry, Università degli Studi di Torino, Via Pietro Giuria 7, 10125 Torino, ItalyDepartment of Chemistry, Università degli Studi di Torino, Via Pietro Giuria 7, 10125 Torino, ItalyThe chemical contamination in fruit and vegetables represents a challenging analytical issue, with tomatoes deserving to be investigated as they are fundamental components of the Mediterranean diet. Polychlorinated biphenyls (PCBs), polycyclic aromatic hydrocarbons (PAHs) and nitro-PAHs contamination is of serious concern, due to particulate deposition and to uptake from contaminated soils and water. However, time-consuming, non-simultaneous and/or non-eco-friendly extraction procedures are typically used to investigate organic contamination in tomatoes, with nitro-PAHs that have not yet been studied. Based on these premises, this work reports the development of a QuEChERS-based approach, coupled with gas chromatography/mass spectrometry, for the simultaneous determination of 16 PAHs, 14 PCBs and 4 nitro-PAHs in three tomato cultivars. The effect of dichloromethane, cyclohexane and acetone, as well as of four clean-up phases were studied through the advanced combination of full factorial experimental design and multiple response optimization approaches. The final protocol, based on cyclohexane extraction followed by a double purification step with primary secondary amine and octadecyl silica and a sulfuric acid oxidation, led to 60–120% recoveries (RSD% < 15%). Good repeatability (inter-day precision <15%) and negligible matrix effect (<16%) were confirmed and the protocol was applied to the analysis of real tomato samples purchased in a local market.https://www.mdpi.com/2297-8739/10/3/174tomatoesfood contaminationorganic micropollutantsPAHPCBnitro-PAH
spellingShingle Luca Rivoira
Massimo Del Bubba
Giasmin Cecconi
Michele Castiglioni
Valentina Testa
Mattia Isola
Maria Concetta Bruzzoniti
Experimental Design and Multiple Response Optimization for the Extraction and Quantitation of Thirty-Four Priority Organic Micropollutants in Tomatoes through the QuEChERS Approach
Separations
tomatoes
food contamination
organic micropollutants
PAH
PCB
nitro-PAH
title Experimental Design and Multiple Response Optimization for the Extraction and Quantitation of Thirty-Four Priority Organic Micropollutants in Tomatoes through the QuEChERS Approach
title_full Experimental Design and Multiple Response Optimization for the Extraction and Quantitation of Thirty-Four Priority Organic Micropollutants in Tomatoes through the QuEChERS Approach
title_fullStr Experimental Design and Multiple Response Optimization for the Extraction and Quantitation of Thirty-Four Priority Organic Micropollutants in Tomatoes through the QuEChERS Approach
title_full_unstemmed Experimental Design and Multiple Response Optimization for the Extraction and Quantitation of Thirty-Four Priority Organic Micropollutants in Tomatoes through the QuEChERS Approach
title_short Experimental Design and Multiple Response Optimization for the Extraction and Quantitation of Thirty-Four Priority Organic Micropollutants in Tomatoes through the QuEChERS Approach
title_sort experimental design and multiple response optimization for the extraction and quantitation of thirty four priority organic micropollutants in tomatoes through the quechers approach
topic tomatoes
food contamination
organic micropollutants
PAH
PCB
nitro-PAH
url https://www.mdpi.com/2297-8739/10/3/174
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