Study Of Analytical Method For Polybrominated Biphenyls And Polybrominated Diphenyl Ethers In Sea Food

Polybrominated Biphenyls (PBBs) and Polybrominated Diphenyl Ethers (PBDEs) have been widely used as a kind of Brominated Flame Retardants (BFRs). They are exploited as additives in Polymers (such as plastics, textiles, electronic equipment and building materials) to prevent ignition and decrease the rate of combustion. They escape to environment from all kinds of synthetical material because they are appended as a kind of flame retardants, and they have a tendency to bioaccumulate in biota and reach humans via the food chain. Due to the wide spread use of PBDEs since1970s, they are ubiquitous in the environment, and rapidly increasing Levels of PBDEs have been detected in the global environment, humans, and other biota. As a result, environmental and biologic pollution induced by them has greatly attracted contemporary world and environmental scientist.To analyze BFR in a great deal of environmental samples, it is urgently needed to develop simple, fast and efficient analytical methods. Gas Chromatography-Mass Spectrometry (GC-EI/MS) is main applied and analytical method now.This thesis focused on study and application of analytical method for PBBs and PBDEs in marine tissue (main fish) by GC-EI/MS. This thesis used Accelerated Solvent Extraction (ASE) as extraction method, the cleanup and separation procedure includes concentrated sulfuric acid and multilayer silica column and established pretreatment method for PBBs and PBDEs in marine tissue, and also optimized ASE conditions on analysis of PBBs and PBDEs in marine tissue. It was validated by analysis of environmental samples at last.The final optimizational conditions of ASE contained:Heat time was5minute; Extraction temperature was70℃; Pressure was1500psi; Static time was6minute; Cycle was2times; Extraction solvent was Hexane/Dichloromethane(1:1, v/v) mixed solvent.The pretreatment method ASE combined with the GC-EI/MS analytical method had applied to the residual analysis of13representative PBBs and PBDEs congeners in marine tissue samples. The linearity was observed in the range of10～200ng ml-1. Coefficient of correlation (r2) ranged from0.9950to0.9996.Method detection limit was between0.44ng g-1and6.0ng g-1(dry weight),the recovery of method were60.8-97.2%, and the RSD values were between1.0%and13.7%, indicating good extraction repeatability. The method was up to the relative standard of EPA.