Quantification of monohydroxy-PAH metabolites in urine by solid-phase extraction with isotope dilution-GC-MS

Anal Bioanal Chem. 2002 Jan;372(1):216-20. doi: 10.1007/s00216-001-1123-8.


For measurement of biomarkers from polycyclic aromatic hydrocarbon (PAH) exposure, an analytical method is described quantifying hydroxylated PAH (OH-PAH) in urine samples. This method determined monohydroxy metabolites of naphthalene, fluorene, phenanthrene, fluoranthene, pyrene, chrysene, benzo[c]phenanthrene, and benz[a]anthracene. The sample preparation consisted of enzymatic hydrolysis, solid-phase extraction and derivatization with a silylating reagent. Five carbon-13 labeled standards were used for isotope dilution. Analytes were separated by gas chromatography (GC) and quantified with high-resolution mass spectrometry (HRMS). This method produced good recoveries (41-70%), linearity, and specificity. Data were corrected for blank levels from the naphthalene, fluorene, and phenanthrene metabolites. Method detection limits ranged from 2 ng L(-1) for 1-hydroxypyrene to 43.5 ng L(-1) for 1-hydroxynaphthalene. Using quality control charts from two urine pools, the method can be readily applied to biomonitoring PAH exposure.

MeSH terms

  • Chromatography, High Pressure Liquid
  • Environmental Monitoring / methods
  • Fluorenes / analysis
  • Gas Chromatography-Mass Spectrometry / methods
  • Humans
  • Hydrolysis
  • Isotope Labeling / methods
  • Mass Spectrometry / methods
  • Naphthalenes / analysis
  • Occupational Exposure
  • Phenanthrenes / analysis
  • Polycyclic Aromatic Hydrocarbons / urine*
  • Pyrenes / analysis
  • Reference Standards
  • Time Factors


  • Fluorenes
  • Naphthalenes
  • Phenanthrenes
  • Polycyclic Aromatic Hydrocarbons
  • Pyrenes
  • naphthalene
  • fluorene
  • phenanthrene
  • 1-hydroxypyrene