Multiclass Multipesticide Residue Analysis in Fish Matrix by a Modified QuEChERS Method Using Gas Chromatography with Mass Spectrometric Determination.
Journal
Journal of AOAC International
ISSN: 1944-7922
Titre abrégé: J AOAC Int
Pays: England
ID NLM: 9215446
Informations de publication
Date de publication:
01 Jan 2020
01 Jan 2020
Historique:
pubmed:
29
8
2019
medline:
29
6
2021
entrez:
29
8
2019
Statut:
ppublish
Résumé
Pesticide residue in fish is a global food safety concern. However, very few validated methods are available targeting simultaneous analysis of multiple classes of pesticides. The aim of this study was to validate a quick, easy, cheap, effective, rugged, and safe workflow-based method for the quantitative determination of multiclass pesticides in fish matrix using GC-MS determination. The sample was extracted with acetonitrile, and the cleanup method involved dispersive solid-phase extraction with C-18 sorbent, which effectively scavenged the coextracted matrix components and removed those from the extract. The data on recovery and precision of the method satisfied the criteria of SANTE/11813/2017 guidelines. Average recoveries of pesticides were in the range of 80-120% with precision RSDs ≤20%. The LOD and LOQ were in the ranges of 0.001-0.029 and 0.005-0.125 µg/mL, respectively, for all pesticides. The expanded uncertainty was in the range of 14-20%, based on the single-laboratory validation data (coverage factor, k = 2, confidence level, 95%). The validation data prove that the method is convenient and acceptable for the routine analysis of multiclass pesticide residues in fish matrices for regulatory compliance. The study achieves multiresidue analysis of pesticides in fish matrix with MS-based confirmation. The method combines the advantages of nontarget analysis based on National Institute of Standards and Technology library matching in full scan mode with selected-ion monitoring-based sensitivity.
Sections du résumé
BACKGROUND
BACKGROUND
Pesticide residue in fish is a global food safety concern. However, very few validated methods are available targeting simultaneous analysis of multiple classes of pesticides.
OBJECTIVE
OBJECTIVE
The aim of this study was to validate a quick, easy, cheap, effective, rugged, and safe workflow-based method for the quantitative determination of multiclass pesticides in fish matrix using GC-MS determination.
METHOD
METHODS
The sample was extracted with acetonitrile, and the cleanup method involved dispersive solid-phase extraction with C-18 sorbent, which effectively scavenged the coextracted matrix components and removed those from the extract. The data on recovery and precision of the method satisfied the criteria of SANTE/11813/2017 guidelines. Average recoveries of pesticides were in the range of 80-120% with precision RSDs ≤20%. The LOD and LOQ were in the ranges of 0.001-0.029 and 0.005-0.125 µg/mL, respectively, for all pesticides. The expanded uncertainty was in the range of 14-20%, based on the single-laboratory validation data (coverage factor, k = 2, confidence level, 95%).
CONCLUSIONS
CONCLUSIONS
The validation data prove that the method is convenient and acceptable for the routine analysis of multiclass pesticide residues in fish matrices for regulatory compliance.
HIGHLIGHTS
CONCLUSIONS
The study achieves multiresidue analysis of pesticides in fish matrix with MS-based confirmation. The method combines the advantages of nontarget analysis based on National Institute of Standards and Technology library matching in full scan mode with selected-ion monitoring-based sensitivity.
Identifiants
pubmed: 31455466
pii: 5717533
doi: 10.5740/jaoacint.19-0205
doi:
Substances chimiques
Pesticide Residues
0
Pesticides
0
Types de publication
Journal Article
Langues
eng
Sous-ensembles de citation
IM
Pagination
62-67Informations de copyright
© AOAC INTERNATIONAL 2020. All rights reserved. For permissions, please email: journals.permissions@oup.com.