Determination of 1-hydroxypyrene in human urine by acid hydrolysis coupled to solid-phase microextraction and semi-microcolumn liquid chromatography.

This study developed an acid hydrolysis coupled to a solid-phase microextraction method employing a semi-microcolumn liquid chromatography system, instead of enzyme hydrolysis with solid-phase extraction for the pretreatment of human urine samples, to detect urinary 1-hydroxypyrene (1-OHP). The complete separation and detection of urinary 1-hydroxyprene was performed using a high-performance liquid-chromatography fluorescence detection system with an analytical C(18) semi-microcolumn, 60% (v/v) aqueous acetonitrile elution, and a lambda(ex/em) = 348/388 nm pair detection wavelength. Calibration graphs were linear with very good correlation coefficients (r = 0.9997), and the detection limit was 1.0 ng/L. These important parameters for acid hydrolysis and solid-phase microextraction were investigated. The total recovery was above 83% in acid hydrolysis with solid-phase microextraction. The proposed method provided a relatively simple, convenient, and practical procedure to determine the level of urinary 1-hydroxypyrene in biological samples, and was successfully applied to detect the urine of students.