소변 중 다환방향족탄화수소 대사체의 분석법 확립 및 교차분석
Method Development and Cross Validation of Analysis of Hydroxylated Polycyclic Aromatic Hydrocarbons (OH-PAHs) in Human Urine
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Objectives: This study was performed to evaluate the analytical method for PAH metabolites in human urineusing 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 foranalysis of 16 OH-PAHs in human urine. Samples were hydrolysis by β-flucuronidase/Aryl sulfatase, and targetcompounds were extracted by solid-phase extraction with a strata-x cartridge. Cross-validation was performedbetween 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) werelower than 10%. The linearity obtained was satisfying for the 16 OH-PAH compounds, with a coefficient ofdetermination (r2) 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.
Abstract
Objectives: This study was performed to evaluate the analytical method for PAH metabolites in human urineusing 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 foranalysis of 16 OH-PAHs in human urine. Samples were hydrolysis by β-flucuronidase/Aryl sulfatase, and targetcompounds were extracted by solid-phase extraction with a strata-x cartridge. Cross-validation was performedbetween 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) werelower than 10%. The linearity obtained was satisfying for the 16 OH-PAH compounds, with a coefficient ofdetermination (r2) 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.
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