Recherche et développement dans le domaine des substances chimiques : préparation aux réponses du sytème REACH

The environment and the health of populations have raised major preoccupations at national level as well as European one. REACH (Registration, Evaluation and Authorization of CHemicals) is a system voted by European Union which brings together more than forty directives in order to eliminate and replace more toxic chemical substances. In this context, the set up of such a system requests robust, reliable and reproducible analytical method to evaluate and detect at ultra-traces level priority substances in waters and soils.After targeting several substances listed on the annexe XVII of REACH, we have completed this selection by other priority pollutants for the environment of “Rhône-Alpes” region, like pesticides. Thus, the analytical method proposed allows the detection and the quantification by GC-MS and LC-MS/MS of 33 substances (10 alkylphenols, 5 triazole fungicides, 1 morpholino fungicides, 1 pyridazinone acaricide, 2 phthalates, bisphenol A, 2 carbamate insecticides, one ditiocarbamates pesticides residu, 2 organophosphorous pesticides and 8 organochlorines) in environmental matrices as complex as wastewater effluents and sludge. The extraction of analytes was led by Solid Phase Extraction (SPE) for aqueous samples and by Accelerated Solvent Extraction (ASE) which was totally optimized by experimental design about parameters. Both extracts were purified by the same way by SPE. The preparation to the validation give us the confirmation of low detection limits comprised between 7.2 ppt and 1.27 ppb in waters and between 5 ppb to 1.7 ppm in sludge/soilsL'environnement et la santé des populations sont devenus des préoccupations majeures aussi bien au niveau national qu'au niveau européen. REACH (Registration, Evaluation and Authorization of CHemicals) est un système adopté par l'Union Européenne qui regroupe plus de quarante directives afin d'éliminer et de remplacer les substances chimiques les plus toxiques. Dans ce contexte, la mise en place d'un tel système requiert des méthodes d'analyse robuste, fiables et reproductibles dans le but d'évaluer et de détecter à l'état d'ultra-traces les molécules prioritaires persistantes dans les eaux et les sols.Après avoir ciblé plusieurs substances listées sur l'annexe XVII de REACH, nous avons complété cette sélection par des polluants prioritaires de l'environnement Rhône Alpin tels les pesticides. Ainsi, la méthode d'analyse proposée permet de détecter et de quantifier par CPG-SM et CPL-SM/SM 33 substances (10 alkylphénols, 5 fongicides triazole, 1 fongicide morpholine, 1 acaricide pyridazinone, 2 phtalates, bisphénol A, 2 insecticides carbamates, un résidu des pesticides dithiocarbamates, 2 pesticides organophosphorés et 8 organochlorés) dans des matrices environnementales aussi complexes que des effluents et des boues de station épuration. L'extraction des analytes est menée par Extraction sur Phase Solide (SPE) pour les échantillons aqueux et par Extraction par Solvant Accélérée (ASE) qui a été entièrement optimisée par étude statistique des paramètres. Les extraits sont ensuite purifiés de la même manière par SPE. La préparation à la validation de ma méthode nous a permis de confirmer des limites de détection basses comprises entre 7,2 ppt et 1,27 ppb dans les eaux et entre 5 ppb et 1,7 ppm dans les boues/sol

Recherche et développement dans le domaine des substances chimiques (préparation aux réponses du sytème REACH)

The environment and the health of populations have raised major preoccupations at national level as well as European one. REACH (Registration, Evaluation and Authorization of CHemicals) is a system voted by European Union which brings together more than forty directives in order to eliminate and replace more toxic chemical substances. In this context, the set up of such a system requests robust, reliable and reproducible analytical method to evaluate and detect at ultra-traces level priority substances in waters and soils. After targeting several substances listed on the annexe XVII of REACH, we have completed this selection by other priority pollutants for the environment of Rhône-Alpes region, like pesticides. Thus, the analytical method proposed allows the detection and the quantification by GC-MS and LC-MS/MS of 33 substances (10 alkylphenols, 5 triazole fungicides, 1 morpholino fungicides, 1 pyridazinone acaricide, 2 phthalates, bisphenol A, 2 carbamate insecticides, one ditiocarbamates pesticides residu, 2 organophosphorous pesticides and 8 organochlorines) in environmental matrices as complex as wastewater effluents and sludge. The extraction of analytes was led by Solid Phase Extraction (SPE) for aqueous samples and by Accelerated Solvent Extraction (ASE) which was totally optimized by experimental design about parameters. Both extracts were purified by the same way by SPE. The preparation to the validation give us the confirmation of low detection limits comprised between 7.2 ppt and 1.27 ppb in waters and between 5 ppb to 1.7 ppm in sludge/soilsLYON1-BU.Sciences (692662101) / SudocSudocFranceF

Determination of nonylphenol and nonylphenol ethoxylates in wastewater using MEKC

Nonylphenol ethoxylates (NPEOx) are surfactants which are used worldwide and can be transformed in the environment by microorganisms to form nonylphenol (NP). Analysis of these compounds was carried out with micellar electrokinetic capillary chromatography (MEKC). Different parameters such as background electrolyte (BGE) solution, pH, type of surfactant, and sample stacking were optimized. The use of CHES (20 mM, pH 9.1) in combination with 50 mM sodium cholate as a surfactant as BGE solution, together with sample stacking using 50 mM NaCl in the sample and an injection time of 20 s, provided the best separation of the compounds studied. The method was applied to the determination of target analytes in two types of sludge water coming from two steps of a wastewater treatment plant. Liquid-liquid extraction was carried out using toluene as solvent, resulting in recoveries around 100% for all studied analytes. The presence of NPEOx was observed in the first step of the sludge water treatment, based on migration time and UV spectra. Identification was confirmed using tandem MS. LOQs of the studied compounds were in the range of 12.7 to 30.8 ng/mL, which is satisfactory for the analysis of real wastewater samples