engleski

Optimization and validation of two-step method for determination of polybrominated diphenyl ethers in Croatian house dust samples

Microwave-assisted extraction was applied as method for extraction of seven polybrominated diphenyl ether (PBDE) congeners (28, 47, 99, 100, 153, 154, and 183) from house dust samples. Optimization of MAE experimental conditions was achieved using a multivariate design approach, and results indicated that only the choice of extraction solvent had a statistically significant influence on extraction efficiency. The extract purification step was also investigated in detail with a goal to achieve an effective cleaning, with minor solvent consumption. As the final operating conditions, 20 min MAE extraction from 1 g of dust with 20 mL of n-hexane:acetone (1:1, v/v) at 80 °C and extract purification on in-lab prepared column containing 2 g of neutral silica and 4 g of acidified silica, whereby the PBDEs were eluted from column with 15 mL of n-hexane:dichloromethane (4:1, v/v), were selected. Extracts were analyzed on dual GC-µECD system, and GC-MS/MS was used as confirmatory method. The performance of the optimized method was validated by analyzing spiked dust samples and a standard reference material (NIST 2585 “Organic Contaminants in House Dust”). Congener specific PBDE recovery ranged from 76 % to 90 % for the spiked samples (with very good repeatability ; RSD < 7 %) and the measured mass concentrations of selected PBDEs were in excellent agreement with certified values for a standard reference material. Proposed method was successfully applied to the analysis of targeted PBDEs in house dust samples.

PBDE, house dust, Croatia

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