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

• Published in: Fēnxī huàxué 2014-09, Vol.42 (9), p.1288-1294
• Main Authors: LI, Min-Jie, JIN, Fen, YANG, Li-Li, WU, Ri-Na, SHAO, Hua, JIN, Mao-Jun, WANG, Jing
• Format: Article
• Language: chi ; eng
• Subjects: Derivatives; Ethers; Gel permeation chromatography; Ionization; Mass spectrometry; Solid phases; Solvent extraction; Spectroscopy
• ISSN: 0253-3820
• DOI: 10.11895/j.issn.0253-3820.140233

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 spectrometrie (HPLC-MS/MS) and gas chromatography-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 C sub(18) dispersive solid phase extraction (SPE) sorbents followed with gel permeation chromatography (GPC), and then analyzed by liquid chromatography tandem mass spectrometrie (HPLC-MS/MS) and gas chromatography-negative chemical ionization mass spectrometry (GC-NCI/MS), respectively. The quantitation 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 mu -g/kg or 5.0 mu g/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 mu g/kg.