Reference : Development and validation of a multi-residue method for pesticide determination in hone...
Scientific journals : Article
Life sciences : Biochemistry, biophysics & molecular biology
Physical, chemical, mathematical & earth Sciences : Chemistry
http://hdl.handle.net/2268/6572
Development and validation of a multi-residue method for pesticide determination in honey using on-column liquid-liquid extraction and liquid chromatography-tandem mass spectrometry
English
Pirard, Catherine [>>]
Widart, Joëlle mailto [Université de Liège - ULg > > Centre interfac. d'analyse des résidus en traces (CART) >]
Nguyen, Bach Kim mailto [Université de Liège - ULg > Gembloux Agro-Bio Tech > Gembloux Agro-Bio Tech >]
Deleuze, Christelle mailto [Université de Liège - ULg > Département de chimie (sciences) > Chimie physique, spectrométrie de masse >]
Heudt, Laetitia mailto [Université de Liège - ULg > > Chimie physique, spectrométrie de masse >]
Haubruge, Eric mailto [Faculté Universitaire des Sciences Agronomiques de Gembloux - FUSAGx > Entomologie fonctionnelle et évolutive > > >]
De Pauw, Edwin mailto [Université de Liège - ULg > > Chimie physique, spectrométrie de masse >]
Focant, Jean-François mailto [Université de Liège - ULg > Département de chimie (sciences) > Chimie analytique - CART > >]
8-Jun-2007
Journal of Chromatography. A
Elsevier Science Bv
1152
1-2
116-123
Yes (verified by ORBi)
International
0021-9673
Amsterdam
Netherland
[en] pesticides ; liquid chromatography ; tandem mass spectrometry ; honey ; diatomaceous earth ; on-column liquid-liquid extraction
[en] We report on the development and validation under ISO 17025 criteria of a multi-residue confirmatory method to identify and quantify 17 widely chemically different pesticides (insecticides: Carbofuran, Methiocarb, Pirimicarb, Dimethoate, Fipronil, Imidacloprid; herbicides: Amidosulfuron, Rimsulfuron, Atrazine, Simazine, Chloroturon, Linuron, Isoxaflutole, Metosulam; fungicides: Diethofencarb) and 2 metabolites (Methiocarb sulfoxide and 2-Hydroxytertbutylazine) in honey. This method is based on an on-column liquid liquid extraction (OCLLE) using diatomaceous earth as inert solid support and liquid chromatography (LC) coupled to mass spectrometry (MS) operating in tandem mode (MS/MS). Method specificity is ensured by checking retention time and theoretical ratio between two transitions from a single precursor ion. Linearity is demonstrated all along the range of concentration that was investigated, from 0.1 to 20 ng g(-1) raw honey, with correlation coefficients ranging from 0.921 to 0.999, depending on chemicals. Recovery rates obtained on home-made quality control samples are between 71 and 90%, well above the range defined by the EC/657/2002 document, but in the range we had fixed to ensure proper quantification, as levels found in real samples could not be corrected for recovery rates. Reproducibility is found to be between 8 and 27%. Calculated CC alpha and CC beta (0.0002-0.943 mg g(-1) for CC alpha, and 0.0002-1.232 ng g(-1) for CCP) show the good sensitivity attained by this rnulti-residue analytical method. The robustness of the method has been tested in analyzing more than 100 raw honey samples collected from different areas in Belgium, as well as some wax and bee samples, with a slightly adapted procedure. (C) 2007 Elsevier B.V. All rights reserved.
Centre Interfacultaire d'Analyse des Résidus en Traces - CART
Région wallonne : Direction générale de l'Agriculture - DGA
http://hdl.handle.net/2268/6572
10.1016/j.chroma.2007.03.035

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