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Por favor, use este identificador para citar o enlazar a este item: http://hdl.handle.net/10261/47886

Determination of pharmaceuticals in soils and sediments by pressurized liquid extraction and liquid chromatography tandem mass spectrometry

AutorVázquez-Roig, Pablo; Segarra, Ramón; Blasco, Cristina; Andreu Pérez, V. ; Picó, Yolanda
Palabras clavePharmaceuticals
Environmental analysis
Liquid chromatography
Tandem mass spectrometry
Solid-phase extraction
Multi-residue method
Fecha de publicación16-abr-2010
CitaciónJournal of Chromatography - A 1217(16): 2471-2483 (2010)
ResumenThe present work describes the development of a sensitive analytical method based on pressurized liquid extraction (PLE) and pre-concentration by solid-phase extraction (SPE), followed by liquid chromatography–electrospray tandem mass spectrometry (LC–ESI-MS/MS) for the determination of seventeen pharmaceuticals in soils and sediments. The method is based on sample homogenisation using Na2–EDTA washed sand and extraction with water at 90 ◦C. Special emphasis was placed on the optimization of the extraction procedure to develop a green method that reduces, at a maximum, the use of organic solvents in order to eliminate matrix components during the clean-up. The proposed method was linear in a concentration range from 0.3 to 333 ng g−1, with correlation coefficients higher than 0.993. Method detection (MDLs) and quantification (MQLs) limits ranged from 0.1 to 6.8 ng g−1 and from 0.25 to 23 ng g−1, respectively. Absolute recoveries were analyte dependent, varying between 50% and 105% at the MQL level, except for fenofibrate (40%) and diclofenac (34%). The intra-day and inter-day precision was given by RSD values from 0.7% to 7.9% and from 1.6% to 14.5%, respectively. Acetaminophen, carbamazepine, ciprofloxacin, clofibric acid, codeine, diazepam, fenofibrate, metropolol, ofloxacin and propanolol were detected at concentrations from MDL to 35.62 ng g−1 in soils and sediments from marsh areas. Due to the low recoveries, results for fenofibrate and diclofenac can only be considered as semi-quantitative. The method was fully suitable for the other 15 pharmaceuticals.
Descripción13 páginas, 4 figuras, 6 tablas.
Versión del editorhttp://dx.doi.org/10.1016/j.chroma.2009.11.033
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