Determination of 1-hydroxypyrene in human urine by HPLC with electrochemical detection at a boron-doped diamond film electrode

摘要

A high-performance liquid chromatographic method with electrochemical detection (HPLC-ED) at a borondoped diamond film electrode with preliminary separation and preconcentration by solid-phase extraction (SPE) has been developed for the determination of 1-hydroxypyrene (1-HP) in human urine. 1-HP is among the most widely used biomarkers of exposure to polycyclic aromatic hydrocarbons. Optimal HPLC-ED conditions have been found: mobile phase methanol-0.05 mol L1 phosphate buffer pH 5.0 (80:20, v/v), detection potential +1,000 mV versus Ag/AgCl (3 mol L1 KCl), and flow rate 0.8 mL min1. For SPE, LiChrolut? RP-18 E cartridges were used. The extraction yield was (87.0±5.8) % (n05). The concentration dependence of 1-HP was measured in the concentration range from 0.01 to 10 μmol L1 (2.18-2,180 μg L1) using methanolic solutions resulting from the SPE pretreatment of spiked human urine samples. The limit of detection (signal-to-noise ratio 3) and the limit of quantification (signal-to-noise ratio 10) of the biomarker were 0.013 μmol L1 (2.84 μg L1) and 0.043 μmol L1 (9.39 μg L1), respectively, which is sufficient for its determination in the urine of persons exposed to polycyclic aromatic hydrocarbons.