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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MDPI AG
2023-03-01
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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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