Determination of 1-hydroxypyrene in human urine by HPLC with electrochemical detection at a boron-doped diamond film electrode.
A high-performance liquid chromatographic method with electrochemical detection (HPLC-ED) at a boron-doped 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 L(-1) phosphate buffer pH 5.0 (80:20, v/v), detection potential +1,000 mV versus Ag/AgCl (3 mol L(-1) KCl), and flow rate 0.8 mL min(-1). For SPE, LiChrolut(®) RP-18 E cartridges were used. The extraction yield was (87.0 ± 5.8)% (n = 5). The concentration dependence of 1-HP was measured in the concentration range from 0.01 to 10 μmol L(-1) (2.18-2,180 μg L(-1)) 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 L(-1) (2.84 μg L(-1)) and 0.043 μmol L(-1) (9.39 μg L(-1)), respectively, which is sufficient for its determination in the urine of persons exposed to polycyclic aromatic hydrocarbons.
Faculty of Science, Department of Analytical Chemistry, UNESCO Laboratory of Environmental Electrochemistry, Charles University in Prague, Prague, Czech Republic. oksana.yosypchuk@seznam.cz
Oksana
O
Yosypchuk
Jiří
J
Barek
Vlastimil
V
Vyskočil
D015415:Biomarkers / Q000652:urine; D001895:Boron / Q000737:chemistry; D002851:Chromatography, High Pressure Liquid / Q000379:methods*; D018130:Diamond / Q000737:chemistry; D055664:Electrochemical Techniques / Q000379:methods*; D004566:Electrodes; D004781:Environmental Exposure; D006801:Humans; D057230:Limit of Detection; D011721:Pyrenes / Q000652:urine*; D059629:Signal-To-Noise Ratio; D052616:Solid Phase Extraction
D015415:Biomarkers; D011721:Pyrenes; D018130:Diamond; C033146:1-hydroxypyrene; D001895:Boron