Determination of 1-Hydroxypyrene as a Biomarker for the Effects of Polycyclic Aromatic Hydrocarbons in Urine by Chromatography–Mass Spectrometry

A simple and sensitive procedure has been developed for the determination of 1-hydroxypyrene in urine as a biological marker of the effects of polycyclic aromatic hydrocarbons. After enzymatic hydrolysis for conjugate cleavage, the analyte was extracted from the matrix by liquid–liquid extraction with n -hexane, the extract was evaporated to dryness, and the analyte was derivatized with the silylating reagent N,O -bis(trimethylsilyl)trifluoroacetamide into trimethylsilyl ether at room temperature. The trimethylsilyl extract was analyzed by capillary gas chromatography with mass-selective detection. Quantitative high-precision determination was achieved with the use of the isotope-labeled 1-hydroxypyrene-d9 reference standard. No matrix effects were observed. The detection limit was 0.02 ng/mL, and the linearity range was 0.1–100 ng/mL. Relative standard deviations were 0.044 and 0.064 under the conditions of repeatability and intralaboratory precision, respectively. The percentage recovery was 96–102%.