Development and Validation of a Rapid Analytical Method for Polybrominated Diphenyl Ethers in House Dust

Abstract

In this study, a rapid analytical method was developed and validated for the determination of polybrominated diphenyl ethers PBDEs in house dust samples. The dust sample was solvent extracted by using a focused ultrasonic processor with reduced extraction time (total 30 min/sample) and solvent volume (about 30 mL/sample). The crude extract was purified by passing through a self-packed multilayer column containing 44% sulfuric acid impregnated silica gel, Florisil, and anhydrous sodium sulfate. PBDEs were eluted from the clean-up column by a mixture of dichloromethane in hexane (1:3,…). PBDEs (41 mono- to deca-BDE congeners) were analyzed by using gas chromatography/mass spectrometry (GC/MS) with negative chemical ionization (NCI) and selected ion monitoring (SIM) mode. The analytical method was validated by using procedural blank, matrix-spike, and standard reference material (SRM) samples. Recoveries of PBDEs in spiked samples ranged from 65% to 120%. Analytical results of the SRM 2585 (Organic Contaminants in House Dust, National Institute of Standards and Technology, USA) indicate method accuracy with ratios of measured to certified values of almost compounds ranging from 76% to 110%. All the experiments were conducted in duplicate, showing acceptable repeatability (RSD < 15%). This method can be applied for simultaneous determination of mono- to deca-BDE congeners in dust samples at ppb to ppm levels with several advantages such as simple, rapid, accurate, cost-effective, and reducing amounts of chemicals and solvents.