Glyphosate and other highly polar pesticides in fruit, vegetables and honey using ion chromatography coupled with high resolution mass spectrometry: Method validation and its applicability in an official laboratory.
glyphosate
high resolution mass spectrometry
ion chromatography
method validation
polar pesticides
Journal
Journal of mass spectrometry : JMS
ISSN: 1096-9888
Titre abrégé: J Mass Spectrom
Pays: England
ID NLM: 9504818
Informations de publication
Date de publication:
Nov 2020
Nov 2020
Historique:
received:
07
02
2020
revised:
10
07
2020
accepted:
11
07
2020
pubmed:
1
8
2020
medline:
3
8
2021
entrez:
1
8
2020
Statut:
ppublish
Résumé
An analytical method, using ion chromatography coupled to high resolution mass spectrometry was developed and validated to quantify glyphosate, glufosinate, ethephon, fosetyl aluminium and their related metabolites. This method allows multiresidue analysis of 11 highly polar molecules in a single chromatographic run, without derivatization step, using acidified water with low level of acetonitrile as extraction solvent. Three different matrices that are representative of commodity group were studied and validated: one fruit (grapes), one cereal (wheat) and honey, according to the criteria established by SANTE/12682/2019 taking into account maximum residue limits indicated by Regulation (EC) No. 396/2005, confirming that the procedure was selective, repeatable and robust. Matrix effect was studied and linearity was evaluated comparing analytical response differences between solvent standard solutions and matrix-matched calibration curve. Due to the relevant matrix effect observed, the use of response factor (RF) approach to quantify analytical batch was evaluated, using isotopically labelled internal standardisation. The in-depth study, validation results and several proficiency tests, used to verify procedure performance, demonstrated that the method is fit for purpose to routine analysis in an official laboratory. Moreover, it allows surveillance activities in fruits and vegetables control, as indicated by European Community, furthermore monitoring presence of polar pesticides, at low level, in some particular food as honey that could become environmental pollution indicator.
Substances chimiques
Pesticides
0
Glycine
TE7660XO1C
Types de publication
Journal Article
Validation Study
Langues
eng
Sous-ensembles de citation
IM
Pagination
e4624Informations de copyright
© 2020 John Wiley & Sons, Ltd.
Références
Benbrook CM. Trends in glyphosate herbicide use in United States and globally. Enviromental Sci Eur. 2016;28(3):1-15.
International Agency for Research on Cancer (IARC). Some organophosate insecticides and herbicides: tetrachlorvinphos, parathion, malathion, diazinon, and glyphosate. 112 Lyon: IARC Working Group; 2015. IARC Monographs on the Evaluation of Carcinogenic Risks to Humans:3-10.
https://www.efsa.europa.eu/it/topics/topic/glyphosate
Bauer N, Kolberg D, Hacker K, Wieland M, Barth A, Anastassiades M. Ethephon-a growth regulator detected in a broad range of crops. European Pesticide Residue Workshop (EPRW) Strasbourg (France), 2010
El-Okazy AM. The effects of combination of gibberellic acid-3 (GA3) and ethephon (2-chloroethyl phosphonic acid) (plant growth regulators) on some physiological parameters in mice. J Egypt Public Health Assoc. 2008;83(1-2):67-86.
Regulation (EC) No. 555/2018 of the European Commission concerning a coordinated multiannual control programme of the Union for 2019, 2020 and 2021 to ensure compliance with maximum residue levels of pesticides and to assess the consumer exposure to pesticide residues in and on food of plant and animal origin
Anastassiades M, Lehotay SJ, Stajnbaher D, Schenck FJ. Fast and easy multiresidue method employing acetonitrile extraction/partitioning and “dispersive solid-phase extraction” for the determination of pesticide residues in produce. J AOAC Int. 2003;86(2):412-431.
Pihlström T, Blomkvist G, Friman P, Pagard U, Österdahl BG. Analysis of pesticide residues in fruit and vegetables with ethyl acetate extraction using gas and liquid chromatography with tandem mass spectrometric detection. Anal Bioanal Chem. 2007;389(6):1773-1789.
Lozano A, Kiedrowska B, Scholten J, de Kroon M, de Kok A, Fernández-Alba AR. Miniaturisation and optimisation of the Dutch mini-Luke extraction method for implementation in the routine multi-residue analysis of pesticides in fruits and vegetables. Food Chem. 2016;192:668-681.
Vass A, Robles-Molina J, Perez-Ortega P, et al. Study of different HILIC, mixed-mode, and other aqueous normal-phase approaches for the liquid chromatography/mass spectrometry-based determination of challenging polar pesticides. Anal Bioanal Chem. 2016;408(18):4857-4869.
Raina-Fulton R. A review of methods for the analysis of orphan and difficult pesticides: glyphosate, glufosinate, quaternary ammonium and phenoxy acid herbicides and dithiocarbamate and phthalimide fungicides. J AOAC Int. 2014;97(4):965-977.
Anastassiades M, Kolberg DI, Eichhorn E, Wachtler AK, Benkenstein A, Zechmann S, Mack D, Wildgrube C, Barth A, Sigalov I, Görlich S, Dörk D, Cerchia G. Quick method for the analysis of numerous highly polar pesticides in food involving extraction with acidified methanol and LC-MS/MS measurement-Food of Plant Origin (QuPPe-PO-Method). EURL Single Residue Methods, Version 10.1 2019.
Qiu H-M, Geng J-J, Han C, Ren HQ. Determination of phosphite, phosphate, glyphosate and aminomethylphosphonic acid by two-dimensional ion chromatography system coupled with capillary ion chromatography. Chin J Anal Chem. 2013;41(12):1910-1914.
Guo Z-X, Cai Q, Yang Z. Determination of glyphosate and phosphate in water by ion chromatography-inductively coupled plasma mass spectrometry detection. J Chromatogr A. 2005;1100(2):160-167.
Lopez-Moreno C, Viera I, Urbano AM. Validation of an ion chromatographic method for the quantification of anions in water. Desalination. 2010;261(1-2):111-116.
Rajski L, Diaz Galiano FJ, Cutillas V, Fernández-Alba AR. Coupling ion chromatography to Q-Orbitrap for the fast and robust analysis of anionic pesticides in fruits and vegetables. J AOAC Int. 2017;101(2):352-359.
Adams S, Guest J, Dickinson M, Fussell RJ, Beck J, Schousten F. Development and validation of ion chromatography-tandem mass spectrometry based method for the multiresidue determination of polar ionic pesticides in food. J Agri Food Chemistr. 2017;65(34):7294-7304.
Bauer A, Luetjohann J, Rohn S, Kuballa J, Jantzen E. Ion chromatography tandem mass spectrometry for the determination of highly polar pesticides in plant derived commodities. Food Control. 2018;86:71-76.
Melton LM, Taylor MJ, Flynn EE. The utilisation of ion chromatography and tandem mass spectrometry (IC-MS/MS) for the multi-residue simultaneous determination of highly polar anionic pesticides in fruit and vegetables. Food Chem. 2019;298:1-8, 125028.
Chesia LM, Nobile M, Panseri S, Arioli F. Detection of glyphosate and its metabolites in food of animal origin based on ion-chromatography-high resolution mass spectrometry (IC-HRMS). Food Addit Contam Part A Chem Anal Control Expo Risk Assess. 2019;36(4):592-600.
Paraja L, Jesùs F, Heinzen H, Hernando MD, Rajski L, Fernández-Alba AR. Evaluation of glyphosate and AMPA in honey by water extraction followed by ion chromatography mass spectrometry. A pilot monitoring study. Anal Methods. 2019;11(16):2123-2128.
SANTE/12682/2019. Guidance document on analytical quality control and method validation procedures for pesticide residues and analysis in food and feed.
Regulation (EC) No 396/2005 of the European Parliament and of the Council of 23 February 2005 on maximum residue levels of pesticides in or on food and feed of plant and animal origin and amending Council Directive 91/414/EECText with EEA relevance.
Botero-Coy AM, Ibáñez M, Sancho JV, Hernández F. Direct liquid chromatography-tandem mass spectrometry determination of underivatized glyphosate in rice, maize and soybean. J Chromatogr A. 2013;1313:157-165.