Abstract
A solid phase extraction-gas chromatography-negative chemical ionization-mass spectrometric method was developed for the simultaneous determination of 2, 3, 5, 6-tetrabromo-P-xylene (pTBX), 1,2,3,4,5-pentabromobenzene (PBBz), Pentabromotoluene (PBT), 2, 3, 5, 5, 6-pentabromoethylbenzene (PBEB), Hexabromobenzene (HBB), sys-Dechlorane Plus (s-DP), anti-Dechlorane Plus (a-DP) and polybrominated diphenyl ethers (PBDEs). Willow bark samples were extracted with hexane-acetone (1: 1, V/V) for 24 h by Soxhlet extraction apparatus and cleaned with a silica/alumina column, which was eluted by hexane :dichloromethane (3 :7). Recoveries in the matrix ranged from 76.2% to 92.3%, and limits of detection were from 0.1 to 5.0 ng/g lipid. Recoveries of C-13(6)-HBB, C-13(12)-BDE-139 and C-13(10)-s-DP in the samples were 75.6% +/- 2.2%, 77.3% +/- 3.4% and 76.0% +/- 2.8%, respectively. pTBX, PBT, PBBz, HBB, s-DP, a-DP and PBDEs were detected in all bark samples, while the detection rate of PBEB was 16.7%.
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