期刊
JOURNAL OF CHROMATOGRAPHY A
卷 1374, 期 -, 页码 85-92出版社
ELSEVIER SCIENCE BV
DOI: 10.1016/j.chroma.2014.11.022
关键词
Organophosphate flame retardants and diesters; LC-ESI-MS/MS; Liver; Egg; Serum; Great Lakes herring gulls
资金
- Environment Canada's Chemicals Management Plan (CMP)
- National Science and Engineering Research Council (NSERC) of Canada [189079]
Environmentally relevant organophosphate (OP) triester flame retardants are known to degrade to OP diester phosphoric acids. In this study, a quantitatively sensitive method was developed for OP diesters in biological samples of varying complexity, bovine serum, chicken egg homogenate and pork liver. Fortified with 1 ng or 10 ng each of the six OP diester and six OP triester standards, samples were extracted by accelerated solvent extraction that completely separated OP diesters and triesters. OP diester fractions were cleaned up using weak anion exchange solid phase extraction and eluted with high ionic strength ammonium acetate buffer. Optimal analysis of chlorinated OP diesters was via decamethonium hydroxide dicationic reagent derivatization and by LC-ESI(+)-MS/MS, and for all non-chlorinated OP diesters by non-derivatized LC-ESI(-)-MS/MS. Except for derivatization LC-ESI(+)-MS/MS analysis of liver, at the long spiking level for the three matrices, recovery efficiencies, matrix effects and method limits of quantification (MLOQs) of OP diesters ranged from 55-116%, 92-119%, and 0.02-0.31 ng/g wet weight (ww) respectively. Plasma samples of n = 6 herring gulls (2010, Chantry Is., Laurentian Great Lakes) contained triphenyl phosphate and tris(1-3-dichloro-2-propyl) phosphate ranging from 1.3 to 4.0 ng/g ww and
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