| Hexabromocyclododecane (HBCD) and Tetrabromobisphenol A (TBBPA) are two new kinds of brominated flame retardands (BFRs). HBCD had been included in the list of Persistent Organic Pollutants (POPs), and TBBPA, which was the maximum yield of brominated flame retardants all over the world, had been considered as an Environmental Endocrine Disruptors(EEDs) in recent years. They have become a hot research topic in the world, because they are now ubiquitous contaminants in wildlife, as well as in humans. However, International Standard Organization (ISO) has not enacted standard test method of HBCD and TBBPA in every kind of sample, there is also no national standard method in China. The existing method of preliminary treatment had been improved and the instrument detection parameters had been optimized, the pollution level of food of animal origin in Hubei had been evaluated in the study. The results are as follows:1. method for the determination of HBCD and TBBPA in food from animal originA method for simultaneous determination of HBCD and TBBPA by stable isotope dilution, silica gel purification, HPLC-MS/MS was established based on the independent analysis methods of the two kinds of compounds. The effects of different sample preparation on the purification were investigated. Mass parameters were optimized. The results showed that the silica gel column could solve the problems of low recovery ratios and simultaneous determination of HBCD and TBBPA. The limits of detection/quantitation of three HBCD isomers, α-HBCD, β-HBCD and γ-HBCD, were 30.6/102,9.5/31.7,17.4/58 respectively. The limit of detection/quantitation of TBBPA was 30.9/103 (pg/g lipid). The recovery of the method was 89.1%-114.0%. This method could save a lot of solvent, and the limit of detection & quantitation, coefficient of recovery and precision could satisfy the requirements of sample analysis. The reliability and accuracy of this method were verified by international comparison of certified reference materials.2. The evaluation of pollution level of food from animal origin in HubeiIt was evaluated that pollution level of HBCD and TBBPA in fish, meat, egg and milk from Hubei. The daily dietary intakes ("reference" male) of TBBPA and ∑HBCD in Hubei province were estimated based on Previous data. The level of ∑HBCD ranged from <LOD-14.6429ng/g lw. The α-HBCD diastereoisomer, was generally the most abundant isomer comparing with β-and γ-HBCD, the relevance ratio> 80%. The level of TBBPA in meat, egg and milk ranged from <LOD-0.8261ng/g lw, the relevance ratio was approximately 20%; level of TBBPA in fish ranged from <LOD-10.2710ng/g lw, the relevance ratio was approximately 70%. Generally speaking, the pollution levels of HBCD and TBBPA in fish are the highest and widest, the average respectively is 1.3860ng/g lw and 1.3555ng/g lw. The EDIHBCD and EDITBBPA for a "reference" man (male adult,63kg bodyweight) are 136.82pg/kg bw/day and 11.41pg/kg bw/day respectively. The pollution level and EDI in Hubei is at the average level in the national scope, and is at low level around the world. |
