Method Development and Cross Validation of Analysis of Hydroxylated Polycyclic Aromatic Hydrocarbons (OH-PAHs) in Human Urine

소변 중 다환방향족탄화수소 대사체의 분석법 확립 및 교차분석

  • Park, Na-Youn (Department of Health, Environment & Safety, Eulji University) ;
  • Jeon, Jung-Dae (Department of Health, Environment & Safety, Eulji University) ;
  • Koo, Hyeryeong (Institute of Metabolism, Green Cross Laboratories) ;
  • Kim, Jung Hoan (Food Technology & Service, Eulji University) ;
  • Lee, Eun-Hee (Graduate School of Health Science, Far-East University) ;
  • Lee, Kyungmu (Department of Environmental Health, Korea National Open University) ;
  • Mun, Cheoljin (Institute of Metabolism, Green Cross Laboratories) ;
  • Kho, Younglim (Department of Health, Environment & Safety, Eulji University)
  • 박나연 (을지대학교 보건환경안전학과) ;
  • 전중대 (을지대학교 보건환경안전학과) ;
  • 구혜령 (녹십자의료재단 대사의학연구소) ;
  • 김정환 (을지대학교 식품산업외식학과) ;
  • 이은희 (극동대학교 보건과학대학원) ;
  • 이경무 (한국방송통신대학교 환경보건학과) ;
  • 문철진 (녹십자의료재단 대사의학연구소) ;
  • 고영림 (을지대학교 보건환경안전학과)
  • Received : 2015.07.09
  • Accepted : 2015.10.15
  • Published : 2015.10.28


Objectives: This study was performed to evaluate the analytical method for PAH metabolites in human urine using enzyme hydrolysis and solid-phase extraction coupled with LC-(ESI)-MS/MS technique. Methods: We employed HPLC tandem mass spectrometry techniques with appropriate pre-treatment for analysis of 16 OH-PAHs in human urine. Samples were hydrolysis by ${\beta}$-flucuronidase/Aryl sulfatase, and target compounds were extracted by solid-phase extraction with a strata-x cartridge. Cross-validation was performed between Eulji University and Green Cross laboratories with 200 human urine samples. Results: The accuracies were between 90.3% and 118.8%, and precisions (relative standard deviations) were lower than 10%. The linearity obtained was satisfying for the 16 OH-PAH compounds, with a coefficient of determination ($r^2$) higher than 0.99. The results of cross-validation at the two organizations were compared by ICC (interclass correlation coefficient) values. The cross-validation results were excellent or good for all compounds. Conclusion: An analytical method was validated for low nanogram levels of 16 OH-PAHs in human urine. Also, satisfying results were obtained for method validation such as accuracy, precision and ICC of cross-validation.


Supported by : 식품의약품안전평가원


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