Determination of pharmaceuticals in soils and sediments by pressurized liquid extraction and liquid chromatography tandem mass spectrometry
| Autor: | Cristina Blasco, Yolanda Picó, Ramón Segarra, Vicente Andreu, Pablo Vázquez-Roig |
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| Přispěvatelé: | Ministerio de Educación y Ciencia (España), European Commission, Ministerio de Ciencia e Innovación (España) |
| Jazyk: | angličtina |
| Rok vydání: | 2010 |
| Předmět: |
Geologic Sediments
Electrospray Tandem mass spectrometry Liquid chromatography Chemical Fractionation Sensitivity and Specificity Biochemistry High-performance liquid chromatography Analytical Chemistry Matrix (chemical analysis) Soil Liquid chromatography–mass spectrometry Antibiotics Soil Pollutants Sample preparation Solid phase extraction Environmental analysis Solid-phase extraction Chromatography Chemistry Organic Chemistry Extraction (chemistry) Reproducibility of Results General Medicine Multi-residue method Pharmaceutical Preparations Linear Models Pharmaceuticals Sediment Chromatography Liquid |
| Zdroj: | Digital.CSIC. Repositorio Institucional del CSIC instname |
| Popis: | 13 páginas, 4 figuras, 6 tablas. The 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. The authors thank the Spanish Ministry of Education and Science together the European Regional Development Funds (ERDF)(projects GCL2007-66687-C02-01/BOS and GLC2008-01693/BTE)for financial support. Pablo Vázquez-Roig is holder of FPI grant from the Ministry of Science and Innovation (MICINN, Spain). |
| Databáze: | OpenAIRE |
| Externí odkaz: |
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