title: Determination of nine hydroxylated polybrominated diphenyl ethers in water by precolumn derivatization-gas chromatography-mass spectrometry.
abstract: Hydroxylated polybrominated diphenyl ethers (OH-PBDEs), acting as emerging endocrine disruptors, have aroused more and more concern recently. Produced from natural source or metabolism of PBDEs, OH-PBDEs are more toxic than their parent compounds. However, few analytical methods are available for sensitive determination of these compounds especially in water. In this study, a method of determination of nine OH-PBDEs in lake, reservoir, river and sewage treatment plant effluent was established using N,O-bis (trimethylsilyl) trifluoroacetamide (BSTFA) as derivatization reagent combined with gas chromatography-mass spectrometry (GC-MS). Optimal extraction solvent and derivatization factors such as the amount of BSTFA, time, temperature and dissolution solvent were determined experimentally. After extracted by hexane-dichloromethane (1:1, v/v), extracts were evaporated to almost dry, then BSTFA was added to the residue and heated at 90°C for 30min. The remains were dried under a stream of nitrogen and redissolved in hexane. The solution was separated in DB-35MS column, then determined by GC-MS in selected ion mode and full scan monitoring mode, and quantified by external standard method. The working curves were obtained using sample matrix in order to eliminate the matrix interference. Linear range was from 0.02μgL(-1) to 30μgL(-1). Limits of detection and quantification ranged from 0.0039μgL(-1) to 0.0220μgL(-1) and 0.0130μgL(-1) to 0.0733μgL(-1), respectively. Two different spiked levels were measured with 5 parallel tests for each level. The results indicated that the relative standard deviations were less than 14.08%. The method has been applied to lake water, reservoir water, river water and sewage treatment plant effluent. Five OH-PBDEs including 2'-OH-BDE3, 3'-OH-BDE7, 2'-OH-BDE28, 4'-OH-BDE17 and 5'-OH-BDE99 were detected in all the samples collected in Baoding, China. This method is simple, high sensitive, and suitable for simultaneous determination of nine OH-PBDEs in different environmental water.
authors.affiliation: College of Chemistry & Environmental Science, No. 180 Wusi East Road, Baoding 071000, China; Key Laboratory of Analytical Science and Technology of Hebei Province, No. 180 Wusi East Road, Baoding 071000, China.
authors.forename: Boqu
authors.initials: B
authors.lastname: Yu
authors.affiliation: College of Chemistry & Environmental Science, No. 180 Wusi East Road, Baoding 071000, China.
authors.forename: Ruirui
authors.initials: R
authors.lastname: Zhang
authors.affiliation: College of Chemistry & Environmental Science, No. 180 Wusi East Road, Baoding 071000, China; Key Laboratory of Analytical Science and Technology of Hebei Province, No. 180 Wusi East Road, Baoding 071000, China. Electronic address: hbupyliu@163.com.
authors.forename: Pengyan
authors.initials: P
authors.lastname: Liu
authors.affiliation: College of Chemistry & Environmental Science, No. 180 Wusi East Road, Baoding 071000, China.
authors.forename: Yajing
authors.initials: Y
authors.lastname: Zhang
authors.affiliation: College of Chemistry & Environmental Science, No. 180 Wusi East Road, Baoding 071000, China.
authors.forename: Yanna
authors.initials: Y
authors.lastname: Zhang
authors.affiliation: College of Chemistry & Environmental Science, No. 180 Wusi East Road, Baoding 071000, China.
authors.forename: Yang
authors.initials: Y
authors.lastname: Bai
mesh_terms: D002681:China; D052244:Endocrine Disruptors / Q000032:analysis*; D005240:Feasibility Studies; D005618:Fresh Water / Q000737:chemistry*; D008401:Gas Chromatography-Mass Spectrometry; D055768:Halogenated Diphenyl Ethers / Q000032:analysis*; D006900:Hydroxylation; D007202:Indicators and Reagents; D060106:Lakes; D045483:Rivers; D012722:Sewage / Q000737:chemistry*; D012997:Solvents; D014297:Trimethylsilyl Compounds; D014874:Water Pollutants, Chemical / Q000032:analysis*
chemical_list: D052244:Endocrine Disruptors; D055768:Halogenated Diphenyl Ethers; D007202:Indicators and Reagents; D012722:Sewage; D012997:Solvents; D014297:Trimethylsilyl Compounds; D014874:Water Pollutants, Chemical; C047270:N,N-bis(trimethylsilyl)-2,2,2-trifluoroacetamide; C039293:trimethylchlorosilane
keywords: Derivatization; Gas chromatography–mass spectrometry; Hydroxylated polybrominated diphenyl ethers; N,O-bis (trimethylsilyl) trifluoroacetamide; Simultaneous determination; Water samples