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Automated On-Line Column-Switching HPLC-MS/MS Method with Peak Focusing for the Determination of Nine Environmental Phenols in Urine
Abstract
We developed a method using isotope dilution on-line solid-phase extraction (SPE) coupled to high-performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) for the determination in urine of nine environmental phenolic compounds: Bisphenol A; 4-tert-octylphenol; o-phenylphenol; 2,4-dichlorophenol; 2,5-dichlorophenol; 2,4,5-trichlorophenol; 2,4,6-trichlorophenol; benzophenone-3 (2-hydroxy-4-metoxybenzophenone); and triclosan (2,4,4'-trichloro-2'-hydroxyphenyl ether). A unique fully automated column-switching system, constructed using 1 autosampler, 2 HPLC pumps, and a 10-port switching valve, was designed to allow for concurrent SPE-HPLC operation with peak focusing. The phenols present in 100 microL of urine were retained and concentrated on a C18 reversed-phase size-exclusion SPE column. Then, the phenols were "back-eluted" from the SPE column and diluted through a mixing Tee before being separated from other urine matrix components using a pair of monolithic HPLC columns. The phenols were detected by negative ion-atmospheric pressure chemical ionization-MS/MS. The efficient preconcentration of the phenols by the SPE column, analyte peak focusing by the dilution, and minimal ion suppression in the LC/MS interface by the buffer-free mobile phases resulted in limits of detection as low as 0.1-0.4 ng/mL for most analytes. The method was validated on spiked pooled urine samples and on urine samples from 30 adults with no known occupational exposure to environmental phenols. The method can be used for quick and accurate analysis of large numbers of samples in epidemiologic studies for assessing the prevalence of human exposure to environmental phenols.
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Cited by
Exposure of the U.S. Population to Bisphenol A and 4- tertiary -Octylphenol: 2003–2004
Calafat, A. M., Ye, X., Wong, L.-Y., Reidy, J. A., & Needham, L. L. (2008) · Environmental Health Perspectives · doi:10.1289/ehp.10753 · Cited by 1,743
Self-citationCorrales, J., Kristofco, L. A., Steele, W. B., Yates, B. S., Breed, C. S., Williams, E. S., & Brooks, B. W. (2015) · Dose-Response · doi:10.1177/1559325815598308 · Cited by 771
Impact of Early-Life Bisphenol A Exposure on Behavior and Executive Function in Children
Braun, J. M., Kalkbrenner, A. E., Calafat, A. M., Yolton, K., Ye, X., Dietrich, K. N., & Lanphear, B. P. (2011) · Pediatrics · doi:10.1542/peds.2011-1335 · Cited by 561
Self-citationPrenatal bisphenol A exposure and early childhood behavior.
Braun, J. M., Yolton, K., Dietrich, K. N., Hornung, R., Ye, X., Calafat, A. M., & Lanphear, B. P. (2009) · Environmental Health Perspectives · doi:10.1289/ehp.0900979 · Cited by 481
Self-citationMeeker, J. D., Ehrlich, S., Toth, T. L., Wright, D. L., Calafat, A. M., Trisini, A. T., Ye, X., & Hauser, R. (2010) · Reproductive Toxicology · doi:10.1016/j.reprotox.2010.07.005 · Cited by 414
Self-citationExposure to Bisphenol A and Other Phenols in Neonatal Intensive Care Unit Premature Infants
Calafat, A. M., Weuve, J., Ye, X., Jia, L. T., Hu, H., Ringer, S., Huttner, K., & Hauser, R. (2009) · Environmental Health Perspectives · doi:10.1289/ehp.0800265 · Cited by 374
Self-citationVariability and predictors of urinary bisphenol A concentrations during pregnancy
Braun, J. M., Kalkbrenner, A. E., Calafat, A. M., Bernert, J. T., Ye, X., Silva, M. J., Barr, D. B., Sathyanarayana, S., & Lanphear, B. P. (2011) · Environmental Health Perspectives · doi:10.1289/ehp.1002366 · Cited by 352
Self-citationPrenatal Bisphenol A Exposure and Child Behavior in an Inner-City Cohort
Perera, F., Vishnevetsky, J., Herbstman, J. B., Calafat, A. M., Xiong, W., Rauh, V., & Wang, S. (2012) · Environmental Health Perspectives · doi:10.1289/ehp.1104492 · Cited by 332
Self-citationWolff, M. S., Teitelbaum, S. L., Pinney, S. M., Windham, G., Liao, L., Biro, F., Kushi, L. H., Erdmann, C., Hiatt, R. A., Rybak, M. E., et al. (2010) · Environmental Health Perspectives · doi:10.1289/ehp.0901690 · Cited by 301
Self-citationTwenty-Four Hour Human Urine and Serum Profiles of Bisphenol A during High-Dietary Exposure
Teeguarden, J. G., Calafat, A. M., Ye, X., Doerge, D. R., Churchwell, M. I., Gunawan, R., & Graham, M. K. (2011) · Toxicological Sciences · doi:10.1093/toxsci/kfr160 · Cited by 215
Self-citationUrinary bisphenol A and hypertension in a multiethnic sample of US adults
Shankar, A., & Teppala, S. (2012) · Journal of Environmental and Public Health · doi:10.1155/2012/481641 · Cited by 162
Cao, X.-L., Zhang, J., Goodyer, C. G., Hayward, S., Cooke, G. M., & Curran, I. H. A. (2012) · Chemosphere · doi:10.1016/j.chemosphere.2012.05.003 · Cited by 93
Metadata
- Authors
- Ye, X., Kuklenyik, Z., Needham, L. L., & Calafat, A. M.
- Venue
- Analytical Chemistry
- Publisher
- American Chemical Society (ACS)
- Published
- 2005-07-15
- Volume
- 77
- Issue
- 16
- Pages
- 5407-5413
- ISSN
- 0003-2700 (ISSN-L)
- 1520-6882
- OpenAlex
- W2083310900
- Cited by
- 412
- References
- 0
- FWCI
- 13.82
- Type
- journal article
- Language
- en
- Open access
- closed
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