title: Analysis of human urine for fifteen phthalate metabolites using automated solid-phase extraction.
abstract: We improved our previous analytical method to measure phthalate metabolites in urine as biomarkers for phthalate exposure by automating the solid-phase extraction (SPE) procedure and expanding the analytical capability to quantify four additional metabolites: phthalic acid, mono-3-carboxypropyl phthalate, mono-isobutyl phthalate (miBP), and monomethyl isophthalate. The method, which involves automated SPE followed by isotope dilution-high performance liquid chromatography (HPLC)-electrospray ionization (ESI)-tandem mass spectrometry (MS), allows for the quantitative measurement of 15 phthalate metabolites in urine with detection limits in the low ng/ml range. SPE automation allowed for the unattended sequential extraction of up to 100 samples at a time, and resulted in an increased sample throughput, lower solvent use, and better reproducibility than the manual SPE. Furthermore, the modified method permitted for the first time, the separation and quantification of mono-n-butyl phthalate (mBP) and its structural isomer miBP. The method was validated on spiked pooled urine samples and on pooled urine samples from persons with no known exposure to phthalates.
authors.affiliation: Division of Laboratory Sciences, National Center for Environmental Health, Centers for Disease Control and Prevention, 4770 Buford Hwy, Mailstop F17, Atlanta, GA 30341, USA.
authors.forename: Manori J
authors.initials: MJ
authors.lastname: Silva
authors.forename: A Ryan
authors.initials: AR
authors.lastname: Slakman
authors.forename: John A
authors.initials: JA
authors.lastname: Reidy
authors.forename: James L
authors.initials: JL
authors.lastname: Preau
authors.forename: Arnetra R
authors.initials: AR
authors.lastname: Herbert
authors.forename: Ella
authors.initials: E
authors.lastname: Samandar
authors.forename: Larry L
authors.initials: LL
authors.lastname: Needham
authors.forename: Antonia M
authors.initials: AM
authors.lastname: Calafat
mesh_terms: D001331:Automation; D006801:Humans; D010795:Phthalic Acids / Q000032:analysis*; D012680:Sensitivity and Specificity; D021241:Spectrometry, Mass, Electrospray Ionization; D014556:Urine / Q000737:chemistry*
chemical_list: D010795:Phthalic Acids; C032279:phthalic acid