Automated solid-phase extraction method for measuring urinary polycyclic aromatic hydrocarbon metabolites in human biomonitoring using isotope-dilution gas chromatography high-resolution mass spectrometry

Lovisa C. Romanoff, Zheng Li, Kisha J. Young, Nelson C. Blakely, Donald George Jr Patterson, Courtney D. Sandau

Research output: Contribution to journalArticle

75 Citations (Scopus)

Abstract

In order to perform comprehensive epidemiological studies where multiple metabolites of several PAHs are measured and compared in low-dose urine samples, fast and robust methods are needed to measure many analytes in the same sample. We have modified a previous method used for measuring polycyclic aromatic hydrocarbon (PAH) metabolites by automating the solid-phase extraction (SPE) and including an additional eight metabolites. We also added seven new carbon-13 labeled standards, which improves the use of isotope-dilution calibration. Our method included enzyme hydrolysis, automated SPE and derivatization with a silylating reagent followed by gas chromatography (GC), coupled with high-resolution mass spectrometry (HRMS). Using this method, we measured 23 metabolites, representing 9 parent PAHs, with detection limits in the low pg/mL range. All steps in the clean-up procedure were optimized individually, resulting in a method that gives good recoveries (69-93%), reproducibility (coefficient of variation for two quality control pools ranged between 4.6 and 17.1%, N > 156), and the necessary specificity. We used the method to analyze nearly 3000 urine samples in the fifth National Health and Nutrition Examination Survey (NHANES 2001-2002).

Original languageEnglish (US)
Pages (from-to)47-54
Number of pages8
JournalJournal of Chromatography B: Analytical Technologies in the Biomedical and Life Sciences
Volume835
Issue number1-2
DOIs
StatePublished - May 1 2006

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Environmental Monitoring
Polycyclic Aromatic Hydrocarbons
Solid Phase Extraction
Metabolites
Isotopes
Gas chromatography
Gas Chromatography
Dilution
Mass spectrometry
Mass Spectrometry
Polycyclic aromatic hydrocarbons
Nutrition Surveys
Nutrition
Quality control
Hydrolysis
Urine
Carbon
Health
Calibration
Recovery

All Science Journal Classification (ASJC) codes

  • Analytical Chemistry
  • Biochemistry
  • Clinical Biochemistry
  • Cell Biology

Cite this

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title = "Automated solid-phase extraction method for measuring urinary polycyclic aromatic hydrocarbon metabolites in human biomonitoring using isotope-dilution gas chromatography high-resolution mass spectrometry",
abstract = "In order to perform comprehensive epidemiological studies where multiple metabolites of several PAHs are measured and compared in low-dose urine samples, fast and robust methods are needed to measure many analytes in the same sample. We have modified a previous method used for measuring polycyclic aromatic hydrocarbon (PAH) metabolites by automating the solid-phase extraction (SPE) and including an additional eight metabolites. We also added seven new carbon-13 labeled standards, which improves the use of isotope-dilution calibration. Our method included enzyme hydrolysis, automated SPE and derivatization with a silylating reagent followed by gas chromatography (GC), coupled with high-resolution mass spectrometry (HRMS). Using this method, we measured 23 metabolites, representing 9 parent PAHs, with detection limits in the low pg/mL range. All steps in the clean-up procedure were optimized individually, resulting in a method that gives good recoveries (69-93{\%}), reproducibility (coefficient of variation for two quality control pools ranged between 4.6 and 17.1{\%}, N > 156), and the necessary specificity. We used the method to analyze nearly 3000 urine samples in the fifth National Health and Nutrition Examination Survey (NHANES 2001-2002).",
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Automated solid-phase extraction method for measuring urinary polycyclic aromatic hydrocarbon metabolites in human biomonitoring using isotope-dilution gas chromatography high-resolution mass spectrometry. / Romanoff, Lovisa C.; Li, Zheng; Young, Kisha J.; Blakely, Nelson C.; Patterson, Donald George Jr; Sandau, Courtney D.

In: Journal of Chromatography B: Analytical Technologies in the Biomedical and Life Sciences, Vol. 835, No. 1-2, 01.05.2006, p. 47-54.

Research output: Contribution to journalArticle

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AU - Romanoff, Lovisa C.

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AU - Blakely, Nelson C.

AU - Patterson, Donald George Jr

AU - Sandau, Courtney D.

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