PMID- 24210890 OWN - NLM STAT- MEDLINE DCOM- 20140527 LR - 20191210 IS - 1873-3778 (Electronic) IS - 0021-9673 (Linking) VI - 1320 DP - 2013 Dec 13 TI - Halogenated phenolic compound determination in plasma and serum by solid phase extraction, dansylation derivatization and liquid chromatography-positive electrospray ionization-tandem quadrupole mass spectrometry. PG - 111-7 LID - S0021-9673(13)01687-7 [pii] LID - 10.1016/j.chroma.2013.10.068 [doi] AB - A robust, sensitive and accurate method was developed for the simultaneous determination in plasma and serum of suite a halogenated phenolic compounds (HPCs) for which several are known to persist in the environment and analytically pure standards are available. Namely, 14 congeners of hydroxylated polybrominated diphenyl ethers (OH-PBDEs), six congeners of hydroxylated polychlorinated biphenyls (OH-PCBs), pentachlorophenol, pentabromophenol and the flame retardant tetrabromobisphenol A (TBBPA). Solid phase extraction (SPE) enriched the target compounds and cleaned up the samples as a result of efficient adsorption on a strong anion-exchange solid phase SPE cartridge (Oasis MAX). After final clean-up the HPCs were derivatized with dansyl chloride and analyzed by liquid chromatography-tandem mass spectrometry with electrospray ionization in positive mode (ESI(+)). Chromatographic separation was achieved on a Luna PFP(2) column (2mmx100mm, 3mum particle size) with mobile phases of water and acetonitrile (both containing 0.1% formic acid). The addition of the dansyl moiety to the HPCs greatly improved analyte sensitivity as the electrospray ionization efficiency was enhanced. Instrument limits of detection (ILODs) for LC-ESI(+)-MS/MS analysis of the HPCs were in the range of 0.01-0.07ng/mL and the method limits of quantification (MLOQs) were in the range of 0.02-0.15ng/g. Recovery efficiencies of the suite of HPCs ranged from 64% to 118% with relative standard deviations from 2% to 12% from fortified bovine serum samples. The method was successfully applied for HPC determination in representative polar bear and snapping turtle plasma samples. CI - Crown Copyright (c) 2013. Published by Elsevier B.V. All rights reserved. FAU - Chu, Shaogang AU - Chu S AD - Ecotoxicology and Wildlife Health Division, Science and Technology Branch, Environment Canada, National Wildlife Research Centre, Carleton University, Ottawa, ON K1A 0H3, Canada. FAU - Letcher, Robert J AU - Letcher RJ LA - eng PT - Journal Article PT - Research Support, Non-U.S. Gov't PT - Validation Study DEP - 20131026 PL - Netherlands TA - J Chromatogr A JT - Journal of chromatography. A JID - 9318488 RN - 0 (Dansyl Compounds) RN - 0 (Halogens) RN - 0 (Phenols) SB - IM MH - Chromatography, Liquid/*methods MH - Dansyl Compounds/*chemistry MH - Halogens/*blood MH - Limit of Detection MH - Phenols/*blood MH - Quality Control MH - Reproducibility of Results MH - Solid Phase Extraction/*methods MH - Spectrometry, Mass, Electrospray Ionization/*methods MH - Tandem Mass Spectrometry/*methods OTO - NOTNLM OT - Dansylation and SPE OT - Halogenated phenolic compounds OT - LC-ESI(+)-MS/MS OT - Plasma EDAT- 2013/11/12 06:00 MHDA- 2014/05/28 06:00 CRDT- 2013/11/12 06:00 PHST- 2013/07/30 00:00 [received] PHST- 2013/10/09 00:00 [revised] PHST- 2013/10/19 00:00 [accepted] PHST- 2013/11/12 06:00 [entrez] PHST- 2013/11/12 06:00 [pubmed] PHST- 2014/05/28 06:00 [medline] AID - S0021-9673(13)01687-7 [pii] AID - 10.1016/j.chroma.2013.10.068 [doi] PST - ppublish SO - J Chromatogr A. 2013 Dec 13;1320:111-7. doi: 10.1016/j.chroma.2013.10.068. Epub 2013 Oct 26.