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Randomized Controlled Trial
. 2011 Oct;401(7):2123-32.
doi: 10.1007/s00216-011-5294-7. Epub 2011 Aug 11.

Analysis of the Flame Retardant Metabolites bis(1,3-dichloro-2-propyl) Phosphate (BDCPP) and Diphenyl Phosphate (DPP) in Urine Using Liquid Chromatography-Tandem Mass Spectrometry

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Free PMC article
Randomized Controlled Trial

Analysis of the Flame Retardant Metabolites bis(1,3-dichloro-2-propyl) Phosphate (BDCPP) and Diphenyl Phosphate (DPP) in Urine Using Liquid Chromatography-Tandem Mass Spectrometry

E M Cooper et al. Anal Bioanal Chem. .
Free PMC article

Abstract

Organophosphate triesters tris(1,3-dichloro-2-propyl) phosphate (TDCPP) and triphenyl phosphate are widely used flame retardants (FRs) present in many products common to human environments, yet understanding of human exposure and health effects of these compounds is limited. Monitoring urinary metabolites as biomarkers of exposure can be a valuable aid for improving this understanding; however, no previously published method exists for the analysis of the primary TDCPP metabolite, bis(1,3-dichloro-2-propyl) phosphate (BDCPP), in human urine. Here, we present a method to extract the metabolites BDCPP and diphenyl phosphate (DPP) in human urine using mixed-mode anion exchange solid phase extraction and mass-labeled internal standards with analysis by atmospheric pressure chemical ionization liquid chromatography tandem mass spectrometry. The method detection limit was 8 pg mL(-1) urine for BDCPP and 204 pg mL(-1) for DPP. Recoveries of analytes spiked into urine ranged from 82 ± 10% to 91 ± 4% for BDCPP and from 72 ± 12% to 76 ± 8% for DPP. Analysis of a small number of urine samples (n=9) randomly collected from non-occupationally exposed adults revealed the presence of both BDCPP and DPP in all samples. Non-normalized urinary concentrations ranged from 46-1,662 pg BDCPP mL(-1) to 287-7,443 pg DPP mL(-1), with geometric means of 147 pg BDCPP mL(-1) and 1,074 pg DPP mL(-1). Levels of DPP were higher than those of BDCPP in 89% of samples. The presented method is simple and sufficiently sensitive to detect these FR metabolites in humans and may be applied to future studies to increase our understanding of exposure to and potential health effects from FRs.

Figures

Fig 1
Fig 1
Structures of organophosphate triester flame retardants, their diester metabolites bis (1,3-dichloro-2-propyl) phosphate (BDCPP) and diphenyl phosphate (DPP) evaluated in this study, and the corresponding internal standards used in the LC/MS-MS analysis.
Fig 2
Fig 2
Example of LC/MS-MS chromatograms of (a) bis (1,3-dichloro-2-propyl) phosphate (BDCPP) and (b) diphenyl phosphate (DPP) in a standard and a urine extract separated on Phenomenex Kinetex XBC18 (100 mm x 2.1 mm; 2.6 μm). Concentrations of BDCPP standard and sample were 9700 pg mL−1 and 7170 pg mL−1, respectively. Concentrations of DPP standard and sample were 4060 pg mL−1 and 2504 pg mL−1, respectively. The volume of extract analyzed was 0.5 mL.
Fig 3
Fig 3
Bis (1,3-dichloro-2-propyl) phosphate (BDCPP) and diphenyl phosphate (DPP) in nine individual urine samples and pooled urine sample (composite of equal volumes of individual samples) presented as concentrations normalized to urine specific gravity. Error bars are standard deviations of triplicate extractions.
Fig 4
Fig 4
Bis (1,3-dichloro-2-propyl) phosphate (BDCPP) (a) and diphenyl phosphate (DPP) (b) in three urine samples collected in glass and plastic containers. Values are concentrations normalized to urine specific gravity. Error bars are standard deviations of triplicate extractions. Samples for which values are significantly different (ANOVA p < 0.05) between glass and plastic containers are notated with an asterisk (*).

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