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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;Jeon, Jung-Dae;Koo, Hyeryeong;Kim, Jung Hoan;Lee, Eun-Hee;Lee, Kyungmu;Mun, Cheoljin;Kho, Younglim
박나연;전중대;구혜령;김정환;이은희;이경무;문철진;고영림

  • Received : 2015.07.09
  • Accepted : 2015.10.15
  • Published : 2015.10.28

Abstract

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.

Keywords

Cross validation;LC-MS/MS;OH-PAHs;urine

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Acknowledgement

Supported by : 식품의약품안전평가원