Optimization and validation of a two-step method for the determination of polybrominated diphenyl ethers in Croatian house dust samples.
Anal Methods
; 13(31): 3504-3510, 2021 08 12.
Article
en En
| MEDLINE
| ID: mdl-34268546
ABSTRACT
Microwave-assisted extraction was applied as a 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 the 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 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 an in-lab prepared column containing 2 g of neutral silica and 4 g of acidified silica, whereby the PBDEs were eluted from the column with 15 mL of n-hexane dichloromethane (4 1, v/v), were selected. The extracts were analyzed on a dual GC-µECD system, and GC-MS/MS was used as a 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. The proposed method was successfully applied to the analysis of targeted PBDEs in house dust samples.
Texto completo:
1
Base de datos:
MEDLINE
Asunto principal:
Polvo
/
Éteres Difenilos Halogenados
Idioma:
En
Revista:
Anal Methods
Año:
2021
Tipo del documento:
Article
País de afiliación:
Croacia