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Title

Comprehensive liquid chromatography–ion-spray tandem mass spectrometry method for the identification and quantification of eight hydroxylated brominated diphenyl ethers in environmental matrices

AuthorsMas García, Sílvia ; Jáuregui, Olga; Rubio, Fernando; Juan, Anna de; Tauler, Romà ; Lacorte Bruguera, Silvia
KeywordsHydroxylated brominated diphenyl ethers (OH-PBDEs)
Liquid chromatography-ion-spray tandem mass spectrometry
Multiple reaction monitoring
Quality parameters
Environmental samples
Issue Date18-May-2007
PublisherJohn Wiley & Sons
CitationJournal of Mass Spectrometry, 42(7): 890-899 (2007)
AbstractWe propose an instrumental method based on liquid chromatography coupled to negative ionspray ionization (ISP(−)) tandem mass spectrometry (MS/MS), for the simultaneous analysis of eight hydroxylated brominated diphenyl ethers (OH-PBDEs) in four different environmental matrices (soil, fish, sludge and particulate matter). The reversed-phase chromatographic separation was performed on a 50 mm Xbridge C18 column, and the compounds were well resolved with a gradient consisting of a ternary mixture of 5 mMammonium acetate, methanol and acetonitrile. Detection was performed in the multiple reaction monitoring (MRM) mode using the [M − H](−) ion as base peak. The fragmentation pathways of the OH-PBDEs varied according to the hydroxyl substitution in the benzene rings and produced characteristic MRM transitions needed for resolving isomeric compounds. The method is acceptable for quantification in the high picogram per gram dry weight (dw) level for allmatrices analyzed. Repeatability and reproducibility tested at 75 pg μl−1 were below 10% using internal standard quantification. The ISP(−) enhancement due to matrix effects was in the 76–132% range and the highest values corresponded to sludge samples. The use of the proposed method based on LC-ISP(−)-MS/MS opens a new way to directly determine OH-PBDEs without the need of derivatization.
Description10 pages, 4 tables, 2 figures.-- PMID: 17511022 [PubMed].
Publisher version (URL)http://dx.doi.org/10.1002/jms.1224
URIhttp://hdl.handle.net/10261/10287
DOIhttp://dx.doi.org/10.1002/jms.1224
ISSN1076-5174
E-ISSN1096-9888
Appears in Collections:(IDAEA) Artículos
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