Simultaneous analysis of phthalate and organophosphate triesters' metabolites in urine -Exposure assessment to plastisizer and flame retardants and their risk o

摘要

Background: We have reported the method to simultaneous analysis of eight metabolites of five phthalates in urine in ISES2012. We have established simultaneous analysis of three metabolites of organophosphate triesters in addition to phthalate metabolites. Methods: Target metabolites were eight phthalate metabolites (MEHP, 5oxo-MEHP, 5cx-MEPP, 2cx-MMHP, MnBP, MBzP, MiBP, and MCPP) and three organophosphate triesters (BEHP metabolite of TEHP,DBP of TBP, and DPhP of TPhP). Sample preparation consists of 1. deconjucation with an enzyme; β-glucuronidase/arylsulfatase, 2. extraction with ethyl acetate, 3. dried by evaporation, 4. derivatization with N-Methyl-N-tert-Butyldimethylsilytrifluoroacetamide (MTBSTFA), and 5. GS/MS(SIM) analysis. A calibration curve was prepared by the simplified method of standard addition, that six different concentrations of standard solutions were spiked in urine (from 0 to 1.0μg/mL). Organophosphate trimesters were administered to mice and three main metabolites were examined. Results: Good linear correlations were obtained for eleven metabolites, and LOQs calculated as 10SD of five repeated measurement of standard solution in urine (0.01μg/mL) were between 0.006 to 0.053μg/mL After deconjucation with an enzyme, concentration of phthalate metabolites were approximately 1.3 times higher than when deconjucation was not performed. On the other hand, concentrations of organophosphate metabolites were same levels at both with and without enzyme treatment.DBP was detected from urine samples of mice administered TBP, as well as DPhP from TPhP administered mice. However, BEHP was not detected from TEHP administered mice urine. Conclusion: Derivatization with MTBSTFA improves analytical sensitivity of simultaneous analysis. This research was supported by Environment Research and Technology Development Fund (C-1151) of the Ministry of the environment, Japan.