Simultaneous determination of trace polybrominated diphenyl ethers in serum using gas chromatography-negative chemical ionization mass spectrometry with simplified sample preparation

Abstract

An improved method with a simple and rapid solid phase extraction procedure for the simultaneous determination of nine common polybrominated diphenyl ethers (PBDEs) in human serum has been established using gas chromatography-negative chemical ionization mass spectrometry. Purification and lipid removal were carried out directly on a solid phase extraction column using water, concentrated sulfuric acid and 10% aqueous methanol, followed by elution with dichloromethane. The eluent was concentrated and then loaded on a short capillary column to detect PBDEs. The results of the spike recovery experiments in fetal bovine serum showed that the average recoveries of the target compounds were between 80.5% and 110.2%. The intraday relative standard deviations were between 1.2% and 9.8%, and the interday relative standard deviations were between 1.8% and 11.1%. The limits of detection for tribromo to nonabromo diphenyl ethers in fetal bovine serum were in the range of 0.208–0.653 ng L⁻¹ and the limits of quantification were in the range of 0.653–1.000 ng L⁻¹. The limit of quantification for BDE-209 was 10.038 ng L⁻¹ and the correlation coefficients in the linear range were greater than 0.997. This method showed good accuracy and precision, and was suitable for the determination of PBDEs in umbilical cord blood samples.