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Determination of 16 phthalate metabolites in urine using automated sample preparation and on-line preconcentration/high-performance liquid chromatography/tandem mass spectrometry.
Anal Chem. 2005 May 01; 77(9):2985-91.AC

Abstract

We developed an on-line solid-phase extraction (SPE) method, coupled with isotope dilution high-performance liquid chromatography/tandem mass spectrometry (HPLC/MS/MS) and with automated sample preparation, to simultaneously quantify 16 phthalate metabolites in human urine. The method requires a silica-based monolithic column for the initial preconcentration of the phthalate metabolites from the urine and a silica-based conventional analytical column for the chromatographic separation of the analytes of interest. It uses small amounts of urine (100 microL), is sensitive (limits of detection range from 0.11 to 0.90 ng/mL), accurate (spiked recoveries are approximately 100%), and precise (the inter- and intraday coefficients of variation are <10%). The method is not labor intensive, and, because pretreatment of the urine samples was performed automatically using an HPLC autosampler, involves minimal sample handling, thus minimizing exposure to hazardous chemicals. The method was validated on spiked, pooled urine samples and on urine samples from 43 adults with no known exposure to phthalates. The high sensitivity and high throughput (HPLC run time, including the preconcentration step, is 27 min) of this analytical method combined with the ease of use and effective automated sample preparation procedure make it suitable for large epidemiological studies to evaluate the prevalence of human exposure to phthalates.

Authors+Show Affiliations

Kato K
Division of Laboratory Sciences, National Center for Environmental Health, Centers for Disease Control and Prevention, 4770 Buford Hwy, Mailstop F17, Atlanta, Georgia 30341, USA.
Silva MJ
No affiliation info available
Needham LL
No affiliation info available
Calafat AM
No affiliation info available

MeSH

AdultChromatography, High Pressure LiquidHumansPhthalic AcidsReproducibility of ResultsSensitivity and SpecificitySolid Phase ExtractionTandem Mass SpectrometryUrinalysis

Pub Type(s)

Journal Article
Research Support, U.S. Gov't, Non-P.H.S.
Research Support, U.S. Gov't, P.H.S.

Language

eng

PubMed ID

15859620

Citation

Kato, Kayoko, et al. "Determination of 16 Phthalate Metabolites in Urine Using Automated Sample Preparation and On-line Preconcentration/high-performance Liquid Chromatography/tandem Mass Spectrometry." Analytical Chemistry, vol. 77, no. 9, 2005, pp. 2985-91.
Kato K, Silva MJ, Needham LL, et al. Determination of 16 phthalate metabolites in urine using automated sample preparation and on-line preconcentration/high-performance liquid chromatography/tandem mass spectrometry. Anal Chem. 2005;77(9):2985-91.
Kato, K., Silva, M. J., Needham, L. L., & Calafat, A. M. (2005). Determination of 16 phthalate metabolites in urine using automated sample preparation and on-line preconcentration/high-performance liquid chromatography/tandem mass spectrometry. Analytical Chemistry, 77(9), 2985-91.
Kato K, et al. Determination of 16 Phthalate Metabolites in Urine Using Automated Sample Preparation and On-line Preconcentration/high-performance Liquid Chromatography/tandem Mass Spectrometry. Anal Chem. 2005 May 1;77(9):2985-91. PubMed PMID: 15859620.
* Article titles in AMA citation format should be in sentence-case
TY - JOUR T1 - Determination of 16 phthalate metabolites in urine using automated sample preparation and on-line preconcentration/high-performance liquid chromatography/tandem mass spectrometry. AU - Kato,Kayoko, AU - Silva,Manori J, AU - Needham,Larry L, AU - Calafat,Antonia M, PY - 2005/4/30/pubmed PY - 2007/2/7/medline PY - 2005/4/30/entrez SP - 2985 EP - 91 JF - Analytical chemistry JO - Anal Chem VL - 77 IS - 9 N2 - We developed an on-line solid-phase extraction (SPE) method, coupled with isotope dilution high-performance liquid chromatography/tandem mass spectrometry (HPLC/MS/MS) and with automated sample preparation, to simultaneously quantify 16 phthalate metabolites in human urine. The method requires a silica-based monolithic column for the initial preconcentration of the phthalate metabolites from the urine and a silica-based conventional analytical column for the chromatographic separation of the analytes of interest. It uses small amounts of urine (100 microL), is sensitive (limits of detection range from 0.11 to 0.90 ng/mL), accurate (spiked recoveries are approximately 100%), and precise (the inter- and intraday coefficients of variation are <10%). The method is not labor intensive, and, because pretreatment of the urine samples was performed automatically using an HPLC autosampler, involves minimal sample handling, thus minimizing exposure to hazardous chemicals. The method was validated on spiked, pooled urine samples and on urine samples from 43 adults with no known exposure to phthalates. The high sensitivity and high throughput (HPLC run time, including the preconcentration step, is 27 min) of this analytical method combined with the ease of use and effective automated sample preparation procedure make it suitable for large epidemiological studies to evaluate the prevalence of human exposure to phthalates. SN - 0003-2700 UR - https://www.unboundmedicine.com/medline/citation/15859620/Determination_of_16_phthalate_metabolites_in_urine_using_automated_sample_preparation_and_on_line_preconcentration/high_performance_liquid_chromatography/tandem_mass_spectrometry_ DB - PRIME DP - Unbound Medicine ER -