Analysis of Free and Bound Residues of Polybrominated Diphenyl Ethers and Tetrabromobisphenol A in Sediment
- VernacularTitle:气相色谱-质谱法检测沉积物中自由态与束缚态多溴联苯醚和四溴双酚-A
- Author:
Xiulan ZHANG
;
Xiaojun LUO
;
Shejun CHEN
;
Bixian MAI
- Publication Type:Journal Article
- Keywords:
Gas chromatography-mass spectrometry;
polybrominated ethers;
tetrabromobisphenol A;
free and bound;
sediment
- From:
Chinese Journal of Analytical Chemistry
2009;37(11):1577-1582
- CountryChina
- Language:Chinese
-
Abstract:
An analysis method was developed for the determination of free and bound fractions of polybromi-nated ethers (PBDEs) and tetrabromobisphenol A (TBBPA) in sediment. The free PBDE and TBBPA were extracted with acetone/hexane ( 1:1) mixed solvent,and the bound fraction was released from the sediment by saponification reaction at 80℃. PBDEs and TBBPA were separated via adjusting pH; PBDEs were determined by GC-negative chemical ionization (NCl)-MS after cleaned up by multilayer silica column,and TBBPA was derivative before pre-separated by acid silica column and finally determined by GC-EI-MS. All of the target compounds were quantitative by internal standard method. The limits of detection of eight low bromina-ted congeners (BDE28,-47,-66,-100,-99,-154,-153 and -183),deca-BDE ( BDE209),and TBBPA were 0.6 - 12.5 pg/g,172 pg/g and 4. 2 pg/g,respectively;This method is reliable and stable. The recoveries of all compounds were ranged from 74% to 106% and the relative standard deviations were below 10%. This method is suitable for the measurement of different forms of PBDEs and TBBPA in sediment under reliable quality assurance and quality control.
