期刊
JOURNAL OF CHROMATOGRAPHY A
卷 1108, 期 2, 页码 158-165出版社
ELSEVIER SCIENCE BV
DOI: 10.1016/j.chroma.2006.01.008
关键词
SPME; organophosphate compounds; flame retardants; plasticizers; water analysis
The feasibility of solid-phase microextraction (SPME) for the determination of several organophosphorus flame retardants and plastizicers in water samples by gas chromatography-nitrooen phosphorous detection (GC-NPD) is evaluated. These compounds have a wide range of polarities and volatilities and require a thorough optimisation of the different SPME parameters. Considering also possible contamination and carryover sources, the best compromise microextraction conditions were found to be direct extraction of 22 ml samples, containing 300 mg/ml of NaCl, with a PDMS-DVB coated fibre at room temperature. Although equilibrium was not achieved, an extraction time of 40 min allowed obtaining a good sensitivity (quantification limits between 0.010 and 0.025 ng/ml), comparable to that achieved by solid-phase extraction (SPE) of I I samples, producing both similar values of precision and accuracy. Furthermore, the SPME method has shown to be free of matrix effects, avoiding the need of employing the standard addition procedure for quantification, and was suitable for the determination of eight of the nine considered compounds. Only tris-(2-ethylhexyl)-phosphate was neither determinable by SPME nor by SPE. Finally, the application of the developed methodolog to the analysis of wastewater samples, showed that important concentrations of these compounds (up to 10 ng/ml) have been detected in treated sewage water, being discharged into the aquatic environment. (c) 2006 Elsevier B.V. All rights reserved.
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