PMID- 26122855 OWN - NLM STAT- MEDLINE DCOM- 20151016 LR - 20191210 IS - 1873-3778 (Electronic) IS - 0021-9673 (Linking) VI - 1406 DP - 2015 Aug 7 TI - Analysis of polybrominated diphenyl ethers and emerging halogenated and organophosphate flame retardants in human hair and nails. PG - 251-7 LID - S0021-9673(15)00819-5 [pii] LID - 10.1016/j.chroma.2015.06.003 [doi] AB - A method for the digestion, extraction, fractionation, and analysis of three classes of flame retardants, including 36 polybrominated diphenyl ethers (PBDEs), 9 halogenated alternative flame retardants (AFRs), and 12 organophosphate esters (OPEs) in human hair and nail samples was developed. The method employed HNO3/H2O2 digestion, liquid-liquid extraction with (4:1 vol) hexane:dichloromethane, fractionation on a 6g column of 2.5% water deactivated Florisil, and analysis by gas chromatographic mass spectrometry. The accuracy and precision of the method was validated using spiked samples of 6 replicates for both hair and nail samples. The method validation results showed good accuracy and precision for all PBDEs except BDE-209, all AFRs except hexabromobenzene (HBB), and all of the 12 OPEs, with average recovery efficiencies>90% and relative standard deviations (RSDs)<10%. The average recovery efficiencies for HBB were between 60% and 86%, with RSDs<10%. BDE-209 had recovery efficiencies of 64% (RSD, 13%) for hair and 71% (RSD, 10%) for nail. This method was applied to analyze 5 human hair and 5 fingernail samples from the general student population at Indiana University Bloomington campus. BDE-47 and BDE-99 were the predominant PBDEs detected in both hair and nail samples, with a concentration range of 11-620 and 4.6-780ng/g (dry weight) in hair and 7.3-43 and 2.1-11ng/g in nails, respectively. Di-(2-ethylhexyl)-tetrabromophthalate (TBPH) and 2-ethylhexyl-2,3,4,5-tetrabromobenzoate (TBB) were detected in all the samples, with concentrations of 20-240 and 11-350ng/g in hair and <17-80 and <9.2-71ng/g in nails, respectively. Among the 12 OPEs analyzed, tris(2-chloroethyl)phosphate (TCEP), tris(1-chloro-2-propyl)phosphate (TCIPP), tris(1,3-dichloro-2-propyl) phosphate (TDCIPP), and triphenyl phosphate (TPHP) were most often detected. The concentrations of these OPEs (summed together) were 1100-3900 and 380-18,000ng/g in hair and nails, respectively. These levels exceed those of both the PBDEs and the AFRs. CI - Copyright (c) 2015 Elsevier B.V. All rights reserved. FAU - Liu, Liang-Ying AU - Liu LY AD - School of Public and Environmental Affairs, Indiana University, Bloomington, IN 47405, United States. FAU - Salamova, Amina AU - Salamova A AD - School of Public and Environmental Affairs, Indiana University, Bloomington, IN 47405, United States. FAU - He, Ka AU - He K AD - School of Public Health, Indiana University, Bloomington, IN 47405, United States. FAU - Hites, Ronald A AU - Hites RA AD - School of Public and Environmental Affairs, Indiana University, Bloomington, IN 47405, United States. Electronic address: HitesR@Indiana.edu. LA - eng PT - Journal Article PT - Research Support, Non-U.S. Gov't PT - Validation Study DEP - 20150609 PL - Netherlands TA - J Chromatogr A JT - Journal of chromatography. A JID - 9318488 RN - 0 (Flame Retardants) RN - 0 (Halogenated Diphenyl Ethers) RN - 0 (Organophosphates) SB - IM MH - *Chemistry Techniques, Analytical MH - Flame Retardants/*analysis MH - Gas Chromatography-Mass Spectrometry MH - Hair/*chemistry MH - Halogenated Diphenyl Ethers/*analysis MH - Halogenation MH - Humans MH - Liquid-Liquid Extraction MH - Nails/*chemistry MH - Organophosphates/analysis MH - Sensitivity and Specificity OTO - NOTNLM OT - Alternative flame retardants OT - Biomonitoring OT - Gas chromatographic mass spectrometry OT - Human hair and nail OT - Organophosphate ester flame retardants OT - Polybrominated diphenyl ethers EDAT- 2015/07/01 06:00 MHDA- 2015/10/17 06:00 CRDT- 2015/07/01 06:00 PHST- 2015/03/02 00:00 [received] PHST- 2015/05/29 00:00 [revised] PHST- 2015/06/01 00:00 [accepted] PHST- 2015/07/01 06:00 [entrez] PHST- 2015/07/01 06:00 [pubmed] PHST- 2015/10/17 06:00 [medline] AID - S0021-9673(15)00819-5 [pii] AID - 10.1016/j.chroma.2015.06.003 [doi] PST - ppublish SO - J Chromatogr A. 2015 Aug 7;1406:251-7. doi: 10.1016/j.chroma.2015.06.003. Epub 2015 Jun 9.