期刊
ANALYTICAL AND BIOANALYTICAL CHEMISTRY
卷 405, 期 1, 页码 401-411出版社
SPRINGER HEIDELBERG
DOI: 10.1007/s00216-012-6453-1
关键词
Pharmaceuticals; Personal care products; Pressurized hot water extraction (PHWE); Stir bar sorptive extraction (SBSE); Gas chromatography-mass spectrometry (GC-MS)
资金
- FPI fellowship
- Consejeria de Economia, Innovacion y Ciencia of the Regional Government of Andalusia
- [RNM 5417]
- [RNM 6613]
This work describes the development, optimization, and validation of a new method for the simultaneous determination of a wide range of pharmaceuticals (beta-blockers, lipid regulatorsaEuro broken vertical bar) and personal care products (fragrances, UV filters, phthalatesaEuro broken vertical bar) in both aqueous and solid environmental matrices. Target compounds were extracted from sediments using pressurized hot water extraction followed by stir bar sorptive extraction. The first stage was performed at 1,500 psi during three static extraction cycles of 5 min each after optimizing the extraction temperature (50-150 A degrees C) and addition of organic modifiers (% methanol) to water, the extraction solvent. Next, aqueous extracts and water samples were processed using polydimethylsiloxane bars. Several parameters were optimized for this technique, including extraction and desorption time, ionic strength, presence of organic modifiers, and pH. Finally, analytes were extracted from the bars by ultrasonic irradiation using a reduced amount of solvent (0.2 mL) prior to derivatization and gas chromatography-mass spectrometry analysis. The optimized protocol uses minimal amounts of organic solvents (< 10 mL/sample) and time (a parts per thousand 8 h/sample) compared to previous existing methodologies. Low standard deviation (usually below 10 %) and limits of detection (sub-ppb) vouch for the applicability of the methodology for the analysis of target compounds at trace levels. Once developed, the method was applied to determine concentrations of these compounds in several types of sample (wastewater, seawater, pore water, and sediment) from Cadiz Bay (SW Spain). To our knowledge, these findings represent the first information available on the presence of some of the target compounds in the marine environment.
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