Method validation for the analysis of 14 pesticides in aqueous matrices by Stir Bar Sorptive Extraction followed by Liquid Chromatography coupled with tandem Mass Spectrometry (SBSE-LD-LC-MS-MS) - INRAE - Institut national de recherche pour l’agriculture, l’alimentation et l’environnement Accéder directement au contenu
Poster De Conférence Année : 2010

Method validation for the analysis of 14 pesticides in aqueous matrices by Stir Bar Sorptive Extraction followed by Liquid Chromatography coupled with tandem Mass Spectrometry (SBSE-LD-LC-MS-MS)

Résumé

The goal of the European Water Framework Directive (WFD, European Commission, 2000) is to obtain a good biological and chemical status for European rivers by 2015. Consequently, the implementation of the WFD leads to an intensification of pollutant monitoring and requires reliable concentration estimates of organic contaminants such as pesticides. For this purpose different strategies can be developed : grab or automated sampling (fractioned, weekly averaged) and passive sampling. The main tools used for the latter strategy are polar organic chemical integrative samplers (POCIS) or semi permeable membrane device (SPMD). Stir bar sorptive extraction (SBSE) is a solvent free sample preparation technique described in the literature to extract organic compounds from aqueous samples by sorption into a thick film of polydimethysiloxane (PDMS) phase on a glass-coated magnet (David and Sandra, 2007). The aim of this work is to develop and validate, according to the French NF T90-210 standard (AFNOR, 2009), a reliable analytical method for the determination of pesticides in surface water. The 14 selected pesticides (azoxystrobin (AZS), chlorfenvinphos (CFV), diflufenican (DFF), dimetomorph (DMM), diuron (DIU), fenitrothion (FNT), isoproturon (IPU), linuron (LINU), norflurazon (NFZ), spiroxamine (SPX), tebuconazole (TBZ), procymidone (PCM), dichloroaniline (DCA) and 3-(3,4-dichlorophenyl)-1-methylurea (DCPMU)) were chosen because they are frequently detected in water samples from vineyard watersheds and because of their various physico-chemical properties. The sample treatment consists of an extraction on SBSE with addition of Sodium Chloride (NaCl) followed by a liquid desorption with a MeOH/ACN (50/50, v/v) mixture. Isoproturon-D6 was used as surrogate standard to overcome matrix effects during the quantification. Liquid chromatography coupled with electrospray tandem mass spectrometry is performed in the multiple-reaction monitoring mode and molecule identities are confirmed by two quantification and confirmation transitions according to the EEC decision 2002/657/CE. Firstly, conservation and stability of these compounds have been studied. The results show that SBSE must be freezed for one week before liquid desorption to improve recoveries. The final extract in organic mobile phase could be stored at 18°C for one month before analysis. These experiments also show that multiple steps of SBSE washing should be added after liquid desorption in order to re-use them without any contamination. Efficiency and repeatability have been evaluated in EvianÒ mineral water spiked at three contamination levels by quintuplet analysis. Recoveries higher than 60% and relative standard deviations lower than 15% have been obtained. Method reaches limits of quantification between 20ng/L and 1µg/L depending on the compound.
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Dates et versions

hal-02593871 , version 1 (15-05-2020)

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Citer

C. Guillemain, Philippe Bados, Marina Coquery, C. Margoum. Method validation for the analysis of 14 pesticides in aqueous matrices by Stir Bar Sorptive Extraction followed by Liquid Chromatography coupled with tandem Mass Spectrometry (SBSE-LD-LC-MS-MS). 6th international workshop on LC/MS for screening and trace level quantitation in environment and food, Feb 2010, Barcelona, Spain. pp.1, 2010. ⟨hal-02593871⟩

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