An optimized method based on MAE-SPE-GC-MS for the analysis of thirteen PBDEs in airborne particles

Abstract

An efficient and reliable analytical method has been developed for the determination of polybrominated diphenyl ethers (PBDEs) in atmospheric particulates collected by ultra-fine glass fibre filters. Thirteen PBDEs in atmospheric particulates were extracted through a developed method and determined by gas chromatography-mass spectrometry (GC-MS). Compared with the classical Soxhlet method and multi-layer silica column purification procedure, the developed method, including microwave assisted extraction (MAE) and solid phase extraction (SPE) procedures, made the pretreatment procedure of atmospheric particulates samples more automatic and faster. The four important conditions of MAE procedure (extraction solvent, solvent volume, extraction temperature and holding time) and three important conditions of SPE procedure (SPE cartridge, elution solvent and pH) were carefully studied and improved. The method achieved good repeatability and reproducibility with RSDs ranging from 2.0% to 11% for all target PBDEs in atmospheric particulate samples. Satisfactory recoveries for spiked particulate samples ranged from 74.0% to 112%. The limits of detection (LOD) and limits of quantification (LOQ) ranges for filter samples were from 0.11 (BDE-17) to 1.23 ng g⁻¹ dw (BDE-209) and from 0.37 (BDE-17) to 4.10 ng g⁻¹ dw (BDE-209), respectively. The developed method has been successfully demonstrated to determine the concentrations of the target PBDEs in atmospheric particulates from one of the state air quality controlling sites in Kunming, China. The results showed that the concentration range of target PBDEs was from 4.97 to 376 ng g⁻¹ dw. BDE-28 (27.9 ng g⁻¹ dw), BDE-71 (35.4 ng g⁻¹ dw), BDE-190 (265.4 ng g⁻¹ dw) and BDE-209 (375.6 ng g⁻¹ dw) were the four dominant PBDEs at the sampling site.