Development of multiple solid phases extraction (MSP2E) of organic micropollutants

Lors de pollutions accidentelles ou d'actes de malveillance au sein des milieux aquatiques, des plans sont mis en place afin d'utiliser tous les recours et les outils nécessaires pour l'évaluation et la caractérisation de la pollution. La procédure standard consiste au prélèvement suivi d'une analyse en laboratoire. Cependant, lors d'une pollution importante, une prise de décision rapide est primordiale. Le projet de thèse s'inscrit dans cette problématique et a consisté au développement d'un analyseur rapide sur site permettant la détection de micropolluants organiques dans l'eau notamment dans le cadre de pollutions accidentelles. Les objectifs ont été de développer une méthode (MSP2E) de pré-concentration et de fractionnement sur des phases solides multiples suivies d'une étape d'élution et d'une détection UV. Les fractions d'élution sont caractéristiques des propriétés physico-chimiques des molécules cibles. Une approche prédictive a été établie permettant de déterminer a priori la fraction dans laquelle les molécules sont éluées. L'exploitation du spectre UV permet de déterminer la (les) molécule(s) présente(s). Une banque de données spectrales a été réalisée afin de répertorier les différentes caractéristiques (physico-chimiques, fraction d'élution, spectre UV) permettant ainsi la reconnaissance d'une molécule. Dans le cadre de ce travail, une centaine de molécules ont été étudiées, seules ou en mélange. Enfin, la méthodologie a également été transposée à une autre application de détermination de produits dopants dans l'urine.In case of accidental or intentional pollution in aquatic environments, plans are implemented to use any and all recourses and tools available in order to evaluate and to characterize pollution. The current method involves a sampling on site followed by laboratory analysis. But, in case of significant pollution, a rapid decision is clearly needed. The thesis project arises in this context and has been the development of a rapid on-site analyzer for the detection of organic micropollutants in water especially in the context of accidental pollution. The aims of this project were to develop a method (MSP2E) of pre-concentration and fractionation of multiple solid phases followed by a elution step and UV detection. Eluting fractions are related to physico-chemical properties of the target compounds. A predictive approach has been established to determine a priori the fraction in which the molecules are eluted. The UV spectrum analysis may identify the molecule in the different fractions. A database was performed to identify the different characteristics (physico-chemical, eluting fraction, UV spectrum) and for the recognition of a molecule. As part of this work, a hundred molecules were studied alone or in mixture. Finally, the methodology has also been transposed to another application for the determination of doping in urine

UV spectra library [chapter 15]

International audienceWith approximately 150 UV–visible spectra of organic and mineral substances this library is not comparable to other UV–vis spectra databases available. If the number of substances is lesser than other databases, the spectra acquisition conditions and the use of data are exclusively oriented to/for water and wastewater quality monitoring. The great majority of spectra of this library were acquired for substances in aqueous solution, chosen for their potential environmental impact, several of them being a part of the list of priority substances. They are grouped into 10 classes of organic substances, plus one group for organic solvents and one group for minerals. In this new edition, more than 30 substances have been included among 14 pesticides and 15 pharmaceuticals and personal-care products

UV Spectra Library

International audienceWith approx. 150 UV-visible spectra of organic and mineral substances this library is not comparable to other UV-vis spectra databases available. If number of substances is lesser than other databases, the spectra acquisition conditions and the use of data are exclusively oriented to/for water and wastewater quality monitoring. The great majority of spectra of this library were acquired for substances in aqueous solution, chosen for their potential environmental impacts, several of them being part of priority list substances. They are grouped into 10 classes of organic substances, plus one group for organic solvents and one group for minerals. In this new edition, more than 30 substances have been included among 14 pesticides and 15 pharmaceuticals and personal care products. © 2017 Elsevier B.V. All rights reserved

Développement d'une méthode d'extraction sur multiples phases solides (MSP2E) de micropolluants organiques

Lors de pollutions accidentelles ou d'actes de malveillance au sein des milieux aquatiques, des plans sont mis en place afin d'utiliser tous les recours et les outils nécessaires pour l'évaluation et la caractérisation de la pollution. La procédure standard consiste au prélèvement suivi d'une analyse en laboratoire. Cependant, lors d'une pollution importante, une prise de décision rapide est primordiale. Le projet de thèse s'inscrit dans cette problématique et a consisté au développement d'un analyseur rapide sur site permettant la détection de micropolluants organiques dans l'eau notamment dans le cadre de pollutions accidentelles. Les objectifs ont été de développer une méthode (MSP2E) de pré-concentration et de fractionnement sur des phases solides multiples suivies d'une étape d'élution et d'une détection UV. Les fractions d'élution sont caractéristiques des propriétés physico-chimiques des molécules cibles. Une approche prédictive a été établie permettant de déterminer a priori la fraction dans laquelle les molécules sont éluées. L'exploitation du spectre UV permet de déterminer la (les) molécule(s) présente(s). Une banque de données spectrales a été réalisée afin de répertorier les différentes caractéristiques (physico-chimiques, fraction d'élution, spectre UV) permettant ainsi la reconnaissance d'une molécule. Dans le cadre de ce travail, une centaine de molécules ont été étudiées, seules ou en mélange. Enfin, la méthodologie a également été transposée à une autre application de détermination de produits dopants dans l'urine.In case of accidental or intentional pollution in aquatic environments, plans are implemented to use any and all recourses and tools available in order to evaluate and to characterize pollution. The current method involves a sampling on site followed by laboratory analysis. But, in case of significant pollution, a rapid decision is clearly needed. The thesis project arises in this context and has been the development of a rapid on-site analyzer for the detection of organic micropollutants in water especially in the context of accidental pollution. The aims of this project were to develop a method (MSP2E) of pre-concentration and fractionation of multiple solid phases followed by a elution step and UV detection. Eluting fractions are related to physico-chemical properties of the target compounds. A predictive approach has been established to determine a priori the fraction in which the molecules are eluted. The UV spectrum analysis may identify the molecule in the different fractions. A database was performed to identify the different characteristics (physico-chemical, eluting fraction, UV spectrum) and for the recognition of a molecule. As part of this work, a hundred molecules were studied alone or in mixture. Finally, the methodology has also been transposed to another application for the determination of doping in urine.RENNES1-Bibl. électronique (352382106) / SudocSudocFranceF

Inter-laboratory exercise on antibiotic drugs analysis in aqueous samples.

International audienceAn inter-laboratory exercise was organized under the PHARMAS EU project, by the Advanced School of Public Health (EHESP), in order to evaluate the performances of analytical methods for the measurement of antibiotics in waters (surface and tap). This is the first time such an exercise on antibiotics has been organized in Europe, using different kinds of analytical methods and devices. In this exercise thirteen laboratories from five countries (Canada, France, Italy, the Netherlands and Portugal) participated, and a total number of 78 samples were distributed. During the exercise, 2 testing samples (3 bottles of each) prepared from tap water and river water, respectively, spiked with antibiotics, were sent to participants and analyzed over a period of one month. A final number of 77 (98.7%) testing samples were considered. Depending on substances studied by each participant, 305 values in duplicate were collected, with the results for each sample being expressed as the target concentration. A statistical study was initiated using 611 results. The mean value, standard deviation, coefficient of variation, standard uncertainty of the mean, median, the minimum and maximum values of each series as well as the 95% confidence interval were obtained from each participant laboratory. In this exercise, 36 results (6% of accounted values) were outliers according to the distribution over the median (box plot). The outlier results were excluded. In order to establish the stability of testing samples in the course of the exercise, differences between variances obtained for every type of sample at different intervals were evaluated. The results showed no representative variations and it can be considered that all samples were stable during the exercise. The goals of this inter-laboratory study were to assess results variability when analysis is conducted by different laboratories, to evaluate the influence of different matrix samples, and to determine the rate at which participating laboratories successfully completed the tests initiated

Automatic and predictive fractionation of organic micropollutants in contaminated water

International audienceEnvironmental context The safeguarding of water supplies and drinking water is a major issue when considering human health risk management. In this context, an automatic and on-site fractionation system for the detection of organic contaminants has been developed. The main goal of this system is to establish an initial diagnosis by identifying a class of substances involved in a case of pollution. Abstract This paper proposes a new approach for the preconcentration, fractionation, prediction and detection of organic micropollutants in water. The main aim of this study was to implement an innovative fractionation method and a prediction model based on the physicochemical properties of compounds and interactions with the sorbent of solid-phase extraction cartridges. Two sorbents (Strata-SAX and Oasis-HLB) and three specific eluting solvents (mixture of methanol and sodium chloride and mixtures of acetonitrile and ultrapure water) were used to separate organic compounds into five specific fractions according to their physicochemical properties (anionic and cationic or neutral compounds with various polarity). More than 75 molecules (43 molecules individually studied and a mixture with 43 molecules, including 11 molecules individually studied) including pesticides, pharmaceuticals, endocrine disruptors and polycyclic aromatic hydrocarbons, with various properties were studied, and the results showed that the elution fraction can be predicted for more than 85% of the compounds. This methodology could simplify the analytical chain by reducing detailed analysis on limited categories of compounds, and could be used for a rapid and on-site screening of organic compounds. © CSIRO 2016