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J Chromatogr A. 2007 Jun 8;1152(1-2):280-6. Epub 2006 Nov 30.

Microwave-assisted extraction of organophosphate flame retardants and plasticizers from indoor dust samples.

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1
Departamento de Química Analítica, Nutrición y Bromatología, Instituto de Investigación y Análisis Alimentario, Universidad de Santiago de Compostela, Santiago de Compostela 15782, Spain.

Abstract

A procedure for the determination of eight organophosphate flame retardants and plasticizers in dust samples is presented. Microwave-assisted extraction and gas chromatography (GC) with nitrogen-phosphorus detection (NPD) were used for sample preparation and analytes quantification, respectively. Influence of different variables (type and volume of organic solvent, temperature, time, agitation, etc.) on the yield of the extraction step was evaluated. The most important factor was the type of solvent, with the highest efficiencies corresponding to acetone. Under final conditions 10 mL of this solvent were employed. The extraction was carried out at 130 degrees C and satisfactory yields, similar to those obtained with the Soxhlet technique, were achieved. Due to the high content of organic carbon in dust samples, primary acetone extracts had to be subjected to intensive clean-up. Dilution with ultrapure water followed by concentration on a reversed-phase sorbent and further purification using silica, allowed a significant reduction of co-extracted interferences. Application of the developed methodology to indoor dust from private houses showed important concentrations of several organophosphate esters. The highest levels, up to 19 microg/g, corresponded to tris(butoxyethyl) phosphate; moreover, average values of two chlorinated compounds, used as flame retardants and considered as the most concerning species in the group, exceeded the 1 microg/g level.

PMID:
17140588
DOI:
10.1016/j.chroma.2006.11.046
[Indexed for MEDLINE]
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