Rapid determination of polybrominated diphenyl ethers (PBDEs) in fish using selective pressurized liquid extraction (SPLE) combined with automated online gel permeation chromatography-gas chromatography mass spectrometry (GPC-GC/MS)

Abstract

A rapid method for the determination of seven predominant polybrominated diphenyl ethers (PBDEs) in fish was developed. The analysis could be completed in 1 h. The PBDEs in the sample were extracted with fat by selective pressurized liquid extraction (SPLE) using acid alumina as a fat retainer. After concentration, the extract was directly injected into online gel permeation chromatography with gas chromatography-mass spectrometry (GPC-GC/MS) in negative chemical ionization (NCI) mode. Method detection limits of seven PBDEs were between 0.002 and 0.005 ng g⁻¹ fat. Quantitative recoveries ranging from 81.9% to 110.3% were obtained by analysis of spiked fish. The relative standard deviations were less than 15% (n = 6). The method was applied to a certified reference material of fish; all results were in the reference ranges. It was shown to be a rapid and reliable alternative in the routine analysis for PBDEs.

Keywords:

• polybrominated diphenyl ethers (PBDEs)
• selective pressurized liquid extraction (SPLE)
• gel permeation chromatography-gas chromatography mass spectrometry (GPC-GC/MS)
• negative chemical ionization (NCI)
• fish

Acknowledgements

This study was supported by the National High-Tech Research Program of China (Grant Number 2006AA06Z403), the National Science and Technology support program of China (Grant Number 2006BAK02A10), and the New Century Talents Scheme (Grant Number 20677032).

Declaration of interest: The authors report no conflicts of interest. The authors alone are responsible for the content and writing of the paper.