title: Stir bar sorptive extraction of parabens, triclosan and methyl triclosan from soil, sediment and sludge with in situ derivatization and determination by gas chromatography-mass spectrometry.
abstract: The aim of this research work was the evaluation of stir-bar sorptive extraction (SBSE) in combination with an in situ derivatization to determine parabens (methylparaben, isopropylparaben, n-propylparaben, butylparaben and benzylparaben), triclosan and methyltriclosan in soil samples. This is the first time that this approach has been applied to the determination of these compounds in soil samples, providing important advantages over conventional extraction techniques, such as minimization of sampling handling, complete elimination of the use of organic solvents and simplification of the analytical procedure with reduced time consumption. The enriched target analytes were desorbed thermally using a thermodesorption system coupled to a gas chromatograph and a mass spectrometer. The optimized derivatization and SBSE extraction conditions, as well as the analytical characteristics of the method were obtained using spiked soil samples. The proposed methodology proved to be easy to use and sensitive, with limits of detection between 80 ng/kg and 1.06 μg/kg, and reproducibility values below 13%. The accuracy of the method was evaluated at two concentration levels, obtaining apparent recoveries between 91% and 110%. The matrix composition significantly influenced the extraction procedure, and a need to adopt a standard additions protocol is apparent. The analytes assayed were determined successfully in different environmental soil samples.
authors.affiliation: Departamento de Química Analítica, Nutrición y Bromatología, Facultad de Ciencias Químicas, Universidad de Salamanca, Salamanca, Spain. anacasas@usal.es
authors.forename: Ana María Casas
authors.initials: AM
authors.lastname: Ferreira
authors.forename: Monika
authors.initials: M
authors.lastname: Möder
authors.forename: M E Fernández
authors.initials: ME
authors.lastname: Laespada
mesh_terms: D005591:Chemical Fractionation / Q000379:methods*; D052244:Endocrine Disruptors / Q000032:analysis / Q000737:chemistry / Q000302:isolation & purification; D008401:Gas Chromatography-Mass Spectrometry / Q000379:methods*; D019015:Geologic Sediments / Q000737:chemistry; D010226:Parabens / Q000032:analysis / Q000737:chemistry* / Q000302:isolation & purification; D015203:Reproducibility of Results; D012680:Sensitivity and Specificity; D012722:Sewage / Q000737:chemistry; D012987:Soil / Q000737:chemistry; D012989:Soil Pollutants / Q000032:analysis / Q000737:chemistry* / Q000302:isolation & purification; D014260:Triclosan / Q000031:analogs & derivatives* / Q000032:analysis / Q000737:chemistry / Q000302:isolation & purification
chemical_list: D052244:Endocrine Disruptors; D010226:Parabens; D012722:Sewage; D012987:Soil; D012989:Soil Pollutants; D014260:Triclosan; C502486:methyl triclosan