Study And Application Of Analytical Method For Polybrominated Diphenyl Ethers And Polybrominated Biphenyls In Both Sediment And Food By Gas Chromatography-Negative Chemical Ionization/Mass Spectrometry

Brominated Flame Retardants (BFR) is an important one in all flame retardants widely used now, Polybrominated Diphenyl Ethers (PBDEs) and Polybrominated Biphenyls (PBBs) plays an important role in BFR. They escape to environment from all kinds of synthetical material because they are appended flame retardants, and their some congeners have biologic accumulation. 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 and electrical and electronic equipments, it is urgently needed to develop simple, fast and efficient analytical methods. Gas Chromatography-Electron Capture Detector (GC-ECD) and Gas Chromatography-Negative Chemical Ionization/Mass Spectrometry (GC-NCI/MS) is main applied and analytical method now.This thesis focused on study and application of analytical method for PBDEs and PBBs in both sediment and food by GC-NCI/MS. This thesis used Ultrasonic Assisted Extraction (UAE) and established pretreatment method for PBDEs and PBBs in both tea leaf and aquicolous propagation, and also optimized Soxhlet Extraction (SE) conditions on analysis of PBDEs and PBBs in sediment. This thesis consisted of five chapters.In the first chapter, the development, classification, research and application of flame retardant was simply represented, the use of BFR and the effect of PBDEs and PBBs to the human health was more introduced. Current progress of PBDEs and PBBs analysis in environmental samples was summarized with emphasis on the application of sample pretreatment technology and main detection methods. Primary imagination and content of this thesis was brought forward.In the second chapter, we discussed pretreatment conditions on analysis of PBDEs and PBBs by GC-NCI/MS, optimized and chose GC-NCI/MS conditions, especially the choice of temperature increasing process. Different ionization manners were simply introduced and compared on analysis of PBDEs and PBBs. Taking PBDE-100 as an example, we also interpreted structure of main negative ions fragment, fracture mechanism and isotopic abundance by NCI/MS Scan.In the third chapter, analytical method for five PBDEs by GC-NCI/MS was established. This chapter optimized pretreatment method on analysis of five PBDEs in tea leaf, chose the best GC and NCI/MS conditions, discussed linear equation, correlation coefficient, method detection limit, average recovery and relative standard deviation for five PBDEs by GC-NCI/MS, and analyzed concentrations of five PBDEs in eight tea leaf.In the fourth chapter, GC-NCI/MS analytical method was applied to the simultaneous determination of ten BFR (five PBDEs and five PBBs) in fish and shellfish. The application of UAE to the determination of PBDEs and PBBs was studied, acidic and neutral silica gel was used as sorbent. This chapter chose the best GC and NCI/MS conditions for ten BFR, discussed linear equation, correlation coefficient, method detection limit, average recovery and relative standard deviation for ten BFR by GC-NCI/MS, and analyzed concentrations of ten BFR in marine fish, freshwater fish and shellfish.In the fifth chapter, GC-NCI/MS analytical method was applied to the simultaneous determination of ten BFR (five PBDEs and five PBBs) in sediment, and GC-ECD was applied to the determination of PBDE-209. SE conditions were optimized on analysis of PBDEs and PBBs in sediment. This chapter chose the best GC and NCI/MS conditions, discussed linear equation, correlation coefficient, method detection limit, average recovery and relative standard deviation for ten BFR by GC-NCI/MS and PBDE-209 by GC-ECD, analyzed concentrations of ten BRF and PBDE-209 in sediments from Xiamen Sea by GC-NCI/MS and GC-ECD.