Improved quantitative detection of 11 urinary phthalate metabolites in humans using liquid chromatography–atmospheric pressure chemical ionization tandem mass spectrometry
Abstract
Phthalates are widely used as industrial solvents and plasticizers, with global use exceeding four million tons per year. We improved our previously developed high-performance liquid chromatography-atmospheric pressure chemical ionization-tandem mass spectrometric (HPLC-APCI-MS/MS) method to measure urinary phthalate metabolites by increasing the selectivity and the sensitivity by better resolving them from the solvent front, adding three more phthalate metabolites, monomethyl phthalate (mMP), mono-(2-ethyl-5-oxohexyl)phthalate (mEOHP) and mono-(2-ethyl-5-hydroxyhexyl)phthalate (mEHHP); increasing the sample throughput; and reducing the solvent usage. Furthermore, this improved method enabled us to analyze free un-conjugated mono-2-ethylhexyl phthalate (mEHP) by eliminating interferences derived from coelution of the glucuronide-bound, or conjugated form, of the mEHP on measurements of the free mEHP. This method for measuring phthalate metabolites in urine involves solid-phase extraction followed by reversed-phase HPLC-APCI-MS/MS using isotope dilution with (13)C(4) internal standards. We further evaluated the ruggedness and the reliability of the method by comparing measurements made by multiple analysts at different extraction settings on multiple instruments. We observed mMP, monoethyl phthalate (mEP), mono-n-butyl phthalate (mBP), monobenzyl phthalate (mBzP), mEHP, mEHHP and mEOHP in the majority of urine specimens analyzed with DEHP-metabolites mEHHP and mEOHP present in…
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Following metabolism, monoesters of phthalates are conjugated with glucuronide or sulfate and excreted in urine.
“following metabolism, monoesters of phthalates are conjugated with glucuronide or sulfate and excreted in urine [139].”
From A Review of Biomonitoring of Phthalate Exposures (2019) · cites this paper as [139]
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A Review of Biomonitoring of Phthalate Exposures
Wang, Y., Zhu, H., & Kannan, K. (2019) · Toxics · doi:10.3390/toxics7020021 · Cited by 755 · see citing works
- Authors
- Silva, M. J., Malek, N. A., Hodge, C. C., Reidy, J. A., Kato, K., Barr, D. B., Needham, L. L., & Brock, J. W.
- Affiliations
- Centers for Disease Control and Prevention (US)
- Corresponding author
- Silva, Manori J
- Venue
- Journal of Chromatography B
- Publisher
- Elsevier BV
- Published
- 2003-06
- Volume
- 789
- Issue
- 2
- Pages
- 393-404
- ISSN
- 1570-0232 (ISSN-L)
- OpenAlex
- W2085930269
- Cited by
- 158
- References
- 0
- Citations by year
- 2026: 1 · 2025: 2 · 2024: 3 · 2023: 6 · 2022: 6 · 2021: 7 · 2020: 3 · 2019: 5 · 2018: 4 · 2017: 3 · 2016: 8 · 2015: 9 · 2014: 6 · 2013: 6 · 2012: 11
- FWCI
- 10.98
- Type
- journal article
- Language
- en
- Open access
- closed
- Locations
- Journal of Chromatography B (publishedVersion)
- PubMed (publishedVersion)
- Topics
- Physical Sciences › Environmental Science › Health, Toxicology and Mutagenesis › Effects and risks of endocrine disrupting chemicals
- Physical Sciences › Chemistry › Analytical Chemistry › Analytical chemistry methods development
- Physical Sciences › Chemistry › Spectroscopy › Analytical Chemistry and Chromatography
- Keywords
- phthalate metabolites, urinary biomonitoring, mono(2-ethylhexyl) phthalate, MEHHP, MEOHP, monomethyl phthalate, monoethyl phthalate, monobenzyl phthalate, mono-n-butyl phthalate, solid-phase extraction, method validation, plasticizer exposure
- MeSH terms
- Atmospheric Pressure, Chromatography, High Pressure Liquid, Humans, Phthalic Acids, Quality Control, Reference Standards, Sensitivity and Specificity, Mass Spectrometry, Reproducibility of Results
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