Comparison of Different d-SPE Sorbent Performances Based on Quick, Easy, Cheap, Effective, Rugged, and Safe (QuEChERS) Methodology for Multiresidue Pesticide Analyses in Rapeseeds

Pesticide extraction in rapeseed samples remains a great analytical challenge due to the complexity of the matrix, which contains proteins, fatty acids, high amounts of triglycerides and cellulosic fibers. An HPLC-MS/MS method was developed for the quantification of 179 pesticides in rapeseeds. The...

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Main Authors: Saida Belarbi, Martin Vivier, Wafa Zaghouani, Aude De Sloovere, Valerie Agasse, Pascal Cardinael
Format: article
Language:EN
Published: MDPI AG 2021
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Online Access:https://doaj.org/article/3cdc9e1e077c4085ac07a498c487b04b
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spelling oai:doaj.org-article:3cdc9e1e077c4085ac07a498c487b04b2021-11-11T18:39:54ZComparison of Different d-SPE Sorbent Performances Based on Quick, Easy, Cheap, Effective, Rugged, and Safe (QuEChERS) Methodology for Multiresidue Pesticide Analyses in Rapeseeds10.3390/molecules262167271420-3049https://doaj.org/article/3cdc9e1e077c4085ac07a498c487b04b2021-11-01T00:00:00Zhttps://www.mdpi.com/1420-3049/26/21/6727https://doaj.org/toc/1420-3049Pesticide extraction in rapeseed samples remains a great analytical challenge due to the complexity of the matrix, which contains proteins, fatty acids, high amounts of triglycerides and cellulosic fibers. An HPLC-MS/MS method was developed for the quantification of 179 pesticides in rapeseeds. The performances of the quick, easy, cheap, effective, rugged, and safe (QuEChERS) method were evaluated using different dispersive solid-phase extraction (d-SPE) sorbents containing common octadecylsilane silica/primary–secondary amine adsorbent (PSA/C18) and new commercialized d-SPE materials dedicated to fatty matrices (Z-Sep, Z-Sep<sup>+</sup>, and EMR-Lipid). The analytical performances of these different sorbents were compared according to the SANTE/12682/2019 document. The best results were obtained using EMR-Lipid in terms of pesticide average recoveries (103 and 70 of the 179 targeted pesticides exhibited recoveries within 70–120% and 30–70%, respectively, with low RSD values). Moreover, the limits of quantification (LOQ) range from 1.72 µg/kg to 6.39 µg/kg for 173 of the pesticides. Only the recovery for tralkoxydim at 10 μg/kg level was not satisfactory (29%). The matrix effect was evaluated and proved to be limited between −50% and 50% for 169 pesticides with this EMR-Lipid and freezing. GC-Orbitrap analyses confirmed the best efficiency of the EMR-Lipid sorbent for the purification of rapeseeds.Saida BelarbiMartin VivierWafa ZaghouaniAude De SloovereValerie AgassePascal CardinaelMDPI AGarticlemultiresidue pesticide analysesrapeseedsQuEChERS extractiondispersive solid-phase extractionHPLC-MS/MSOrganic chemistryQD241-441ENMolecules, Vol 26, Iss 6727, p 6727 (2021)
institution DOAJ
collection DOAJ
language EN
topic multiresidue pesticide analyses
rapeseeds
QuEChERS extraction
dispersive solid-phase extraction
HPLC-MS/MS
Organic chemistry
QD241-441
spellingShingle multiresidue pesticide analyses
rapeseeds
QuEChERS extraction
dispersive solid-phase extraction
HPLC-MS/MS
Organic chemistry
QD241-441
Saida Belarbi
Martin Vivier
Wafa Zaghouani
Aude De Sloovere
Valerie Agasse
Pascal Cardinael
Comparison of Different d-SPE Sorbent Performances Based on Quick, Easy, Cheap, Effective, Rugged, and Safe (QuEChERS) Methodology for Multiresidue Pesticide Analyses in Rapeseeds
description Pesticide extraction in rapeseed samples remains a great analytical challenge due to the complexity of the matrix, which contains proteins, fatty acids, high amounts of triglycerides and cellulosic fibers. An HPLC-MS/MS method was developed for the quantification of 179 pesticides in rapeseeds. The performances of the quick, easy, cheap, effective, rugged, and safe (QuEChERS) method were evaluated using different dispersive solid-phase extraction (d-SPE) sorbents containing common octadecylsilane silica/primary–secondary amine adsorbent (PSA/C18) and new commercialized d-SPE materials dedicated to fatty matrices (Z-Sep, Z-Sep<sup>+</sup>, and EMR-Lipid). The analytical performances of these different sorbents were compared according to the SANTE/12682/2019 document. The best results were obtained using EMR-Lipid in terms of pesticide average recoveries (103 and 70 of the 179 targeted pesticides exhibited recoveries within 70–120% and 30–70%, respectively, with low RSD values). Moreover, the limits of quantification (LOQ) range from 1.72 µg/kg to 6.39 µg/kg for 173 of the pesticides. Only the recovery for tralkoxydim at 10 μg/kg level was not satisfactory (29%). The matrix effect was evaluated and proved to be limited between −50% and 50% for 169 pesticides with this EMR-Lipid and freezing. GC-Orbitrap analyses confirmed the best efficiency of the EMR-Lipid sorbent for the purification of rapeseeds.
format article
author Saida Belarbi
Martin Vivier
Wafa Zaghouani
Aude De Sloovere
Valerie Agasse
Pascal Cardinael
author_facet Saida Belarbi
Martin Vivier
Wafa Zaghouani
Aude De Sloovere
Valerie Agasse
Pascal Cardinael
author_sort Saida Belarbi
title Comparison of Different d-SPE Sorbent Performances Based on Quick, Easy, Cheap, Effective, Rugged, and Safe (QuEChERS) Methodology for Multiresidue Pesticide Analyses in Rapeseeds
title_short Comparison of Different d-SPE Sorbent Performances Based on Quick, Easy, Cheap, Effective, Rugged, and Safe (QuEChERS) Methodology for Multiresidue Pesticide Analyses in Rapeseeds
title_full Comparison of Different d-SPE Sorbent Performances Based on Quick, Easy, Cheap, Effective, Rugged, and Safe (QuEChERS) Methodology for Multiresidue Pesticide Analyses in Rapeseeds
title_fullStr Comparison of Different d-SPE Sorbent Performances Based on Quick, Easy, Cheap, Effective, Rugged, and Safe (QuEChERS) Methodology for Multiresidue Pesticide Analyses in Rapeseeds
title_full_unstemmed Comparison of Different d-SPE Sorbent Performances Based on Quick, Easy, Cheap, Effective, Rugged, and Safe (QuEChERS) Methodology for Multiresidue Pesticide Analyses in Rapeseeds
title_sort comparison of different d-spe sorbent performances based on quick, easy, cheap, effective, rugged, and safe (quechers) methodology for multiresidue pesticide analyses in rapeseeds
publisher MDPI AG
publishDate 2021
url https://doaj.org/article/3cdc9e1e077c4085ac07a498c487b04b
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