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Communication Dans Un Congrès Année : 2012

Innovative sample preparation steps for the analysis of pharmaceuticals in soil.

Résumé

Chemical products are more and more used for agriculture and domestic activities and are responsible for the spread of several substances in the environment, which can be harmful for animals or humans. Among these products, hormonal steroids and pharmaceutical compounds are of growing concern. If several analytical methods are available to determine the content of these compounds in aquatic environment, few methods were described to allow their analysis in solid matrices. However, the few available data concerning the content of hormonal steroids in soil reveal contaminations which can reach hundreds of ng/kg. Consequently, the aim of this study was to develop an analytical method for the analysis of traces of 11 hormonal steroids, 16 veterinary or human drugs and 11 other well-known human contaminants, used in this study as pollution tag, in soil. An analytical method both selective and sensitive based on liquid chromatography-tandem mass spectrometry was developed. The optimization allowed the determination of the best conditions for the separation by chromatography and for the detection by mass spectrometry. The analysis of complex matrix such as soil needed a rigorous sample preparation to obtain a repeatable and enough sensitive analysis to achieve the detection limits required. For this purpose, an extraction step using the QuEChERS (Quick, Easy, Cheap, Effective, Rugged and Safe) method was set up. This is a relatively new technique, simple, quick and cheap. The use of this method for environmental matrices such as soil is particularly innovative. This technique is based on a liquid-liquid extraction with an organic solvent in presence of salts and buffers. Several parameters were optimized (sample weight, solvent nature, water and solvent volumes, buffer type). A further purification step was necessary to reduce the matrix effects, therefore the SAX (Strong Anion Exchange) cartridge was used in tandem with the Strata-X cartridge for the clean-up. This analytical procedure allows the determination of the target analytes in the lower ng/g range. After a validation based on the ICH/2005 norm, this analytical methodology was successfully applied to real samples of soil collected in several areas of France that were treated differently. Some of them were contaminated with manure spreading, others with sludge spreading and others with atmospheric fallouts. Results indicate that all the samples contained several contaminants at level lower than the ng/g.
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Dates et versions

hal-00704544 , version 1 (05-06-2012)

Identifiants

  • HAL Id : hal-00704544 , version 1

Citer

Marie-Virginie Salvia, Julien Camilleri, Emmanuelle Vulliet, Laure Wiest, Robert Baudot, et al.. Innovative sample preparation steps for the analysis of pharmaceuticals in soil.. 6th SETAC World Congress / SETAC Europe 22nd Annual Meeting, May 2012, Berlin, Germany. ⟨hal-00704544⟩
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