Determination of nine hydroxylated polybrominated diphenyl ethers in water by precolumn derivatization-gas chromatography–mass spectrometry

摘要: Hydroxylated polybrominated diphenyl ethers (OH-PBDEs), acting as emerging endocrine disruptors, have aroused more and concern recently. Produced from natural source or metabolism of PBDEs, OH-PBDEs are toxic than their parent compounds. However, few analytical methods available for sensitive determination these compounds especially in water. In this study, a method nine lake, reservoir, river sewage treatment plant effluent was established using N,O-bis (trimethylsilyl) trifluoroacetamide (BSTFA) derivatization reagent combined with gas chromatography-mass spectrometry (GC-MS). Optimal extraction solvent factors such the amount BSTFA, time, temperature dissolution were determined experimentally. After extracted by hexane-dichloromethane (1:1, v/v), extracts evaporated to almost dry, then BSTFA added residue heated at 90°C 30min. The remains dried under stream nitrogen redissolved hexane. solution separated DB-35MS column, GC-MS selected ion mode full scan monitoring mode, quantified external standard method. working curves obtained sample matrix order eliminate interference. Linear range 0.02μgL(-1) 30μgL(-1). Limits detection quantification ranged 0.0039μgL(-1) 0.0220μgL(-1) 0.0130μgL(-1) 0.0733μgL(-1), respectively. Two different spiked levels measured 5 parallel tests each level. results indicated that relative deviations less 14.08%. has been applied lake water, reservoir water effluent. Five including 2'-OH-BDE3, 3'-OH-BDE7, 2'-OH-BDE28, 4'-OH-BDE17 5'-OH-BDE99 detected all samples collected Baoding, China. This is simple, high sensitive, suitable simultaneous environmental