PMID- 26686560 OWN - NLM STAT- MEDLINE DCOM- 20160725 LR - 20181202 IS - 1873-3778 (Electronic) IS - 0021-9673 (Linking) VI - 1426 DP - 2015 Dec 24 TI - Determination of organophosphate diesters in urine samples by a high-sensitivity method based on ultra high pressure liquid chromatography-triple quadrupole-mass spectrometry. PG - 154-60 LID - S0021-9673(15)01626-X [pii] LID - 10.1016/j.chroma.2015.11.018 [doi] AB - Organophosphate (OP) diesters in urine samples have potential use as biomarkers of organism exposure to environmentally relevant OP triester precursors and in particular OP triester flame retardants. This present study developed a quantitatively sensitive ultra high pressure liquid chromatography (UHPLC-MS) based method for urine and the determination of OP diesters (i.e. diphenyl phosphate (DPHP), bis(2-chloroethyl) phosphate (BCEP), bis(2-chloroisopropyl) phosphate (BDCIPP), di-n-butyl phosphate (DNBP), di(2-ethylhexyl) phosphate (DEHP), bis(1-chloro-2-propyl) phosphate (BCIPP), and bis(2-butoxyethyl) phosphate (BBOEP)). Fortified with the 7 OP diesters, 1mL of human urine sample was cleaned up using weak anion exchange solid phase extraction and eluted with high ionic strength ammonium acetate buffer. Subsequently, 4 non-chlorinated OP diesters were directly determined using UHPLC-electrospray(-)-triple quadrupole-MS (UHPLC-ESI(-)-QqQ-MS), and UHPLC-ESI(+)-QqQ-MS was used for determination of 3 chlorinated OP diesters after methylation using diazomethane. Recovery efficiencies of OP diesters ranged from 88 to 160% at three spiking levels (0.4, 2 and 10ng/mL urine). Matrix effects (MEs) and method limits of quantification (MLOQs) were 15-134% and 0.10-0.32ng/mL urine, respectively. Concentrations of OP diesters in n=12 urine samples (from 4 Canadian residents, 2014) varied as follows, nd-<0.28 (DNBP), nd-1.29 (DPHP), nd-<0.28 (DEHP), <0.16-12.33 (BCEP), nd-1.17 (BCDIPP) and nd-0.68ng/mL (BCIPP). CI - Copyright (c) 2015. Published by Elsevier B.V. FAU - Su, Guanyong AU - Su G AD - Department of Chemistry, Carleton University, Ottawa, ON, Canada K1S 5B6. Electronic address: guanyong.su85@gmail.com. FAU - Letcher, Robert J AU - Letcher RJ AD - Department of Chemistry, Carleton University, Ottawa, ON, Canada K1S 5B6. Electronic address: robert.letcher@canada.ca. FAU - Yu, Hongxia AU - Yu H AD - State Key Laboratory of Pollution Control and Resource Reuse & School of the Environment, Nanjing University, Nanjing, China. LA - eng PT - Journal Article PT - Research Support, Non-U.S. Gov't DEP - 20151110 PL - Netherlands TA - J Chromatogr A JT - Journal of chromatography. A JID - 9318488 RN - 0 (Buffers) RN - 0 (Esters) RN - 0 (Flame Retardants) RN - 0 (Organophosphates) SB - IM MH - Buffers MH - Chromatography, High Pressure Liquid/methods MH - Esters MH - Flame Retardants/analysis MH - Humans MH - Organophosphates/*urine MH - Osmolar Concentration MH - Solid Phase Extraction MH - Spectrometry, Mass, Electrospray Ionization OTO - NOTNLM OT - Canadian residents OT - Organophosphate diesters OT - Organophosphate flame retardants OT - UHPLC-ESI-QqQ-MS OT - Urine EDAT- 2015/12/22 06:00 MHDA- 2016/07/28 06:00 CRDT- 2015/12/22 06:00 PHST- 2015/07/02 00:00 [received] PHST- 2015/10/14 00:00 [revised] PHST- 2015/11/05 00:00 [accepted] PHST- 2015/12/22 06:00 [entrez] PHST- 2015/12/22 06:00 [pubmed] PHST- 2016/07/28 06:00 [medline] AID - S0021-9673(15)01626-X [pii] AID - 10.1016/j.chroma.2015.11.018 [doi] PST - ppublish SO - J Chromatogr A. 2015 Dec 24;1426:154-60. doi: 10.1016/j.chroma.2015.11.018. Epub 2015 Nov 10.