Determination of Polybrominated Diphenyl Ethers and Derivatives, Tetrabromobisphenol A, Hexabromocyclododecane in Egg Samples by Gel Permeation Chromatography and Dispersive Solid Phase Extraction / 分析化学

ABSTRACT

A stimulate method for determination of polybrominated diphenyl ethers ( PBDEs) and derivatives (OH-PBDEs and MeO-PBDEs), tetrabromobisphenol A (TBBPA), hexabromocyclododecane (HBCD) in egg samples was developed by gel permeation chromatography ( GPC) and dispersive solid phase extraction ( DSPE) combined with liquid chromatography tandem mass spectrometric ( HPLC-MS/MS) and gas chroma-tography-negative chemical ionization mass spectrometry ( GC-NCI/MS ) . The analytes were extracted with mixture of hexane and dichloromethane (1∶1, V/V) by accelerated solvent extraction (ASE), and purified by 100 mg C18 dispersive solid phase extraction ( SPE) sorbents followed with gel permeation chromatography (GPC) , and then analyzed by liquid chromatography tandem mass spectrometric (HPLC-MS/MS) and gas chromatography-negative chemical ionization mass spectrometry (GC-NCI/MS), respectively. The quantita-tion was carried out external standard method. The recoveries of objects were 64. 5%-97. 2% and 65. 6%-109 . 2% ( except BDE85 was 54 . 8%, OH-BDE-137 was 47 . 4%) spiked at 1 . 0 μg/kg or 5 . 0 μg/kg in egg white and egg yolk, respectively. The relative standard deviations (RSDs) were less than 20. 2%. The limits of quantitation (LOQ) for the object were 0. 01-0. 2 μg/kg.