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Sample preparation techniques using solid-phase extraction (SPE) and solid-phase microextraction (SPME) are compared for the analysis of monohydroxy polycyclic aromatic hydrocarbons (OHPAH) in human urine. Urine samples spiked with five carbon-13 labeled internal standards are first enzymatically hydrolyzed. Sixteen OHPAH from eight parent compounds (naphthalene, fluorene, phenanthrene, fluoranthene, pyrene, chrysene, benzo[ c ]phenanthrene, and benz[ a ]anthracene) are then extracted along with the internal standards by these two different techniques. The analytes are derivatized by a silylating reagent before final analysis. Final separation and detection are performed by temperature-programmed capillary gas chromatography (GC) and high-resolution mass spectrometry (HRMS). The two extraction techniques are compared for sample preparation time, cost, throughput, reinjection possibility, frequency of outliers, matrix interference, signal linearity, and method detection limit. SPE demonstrates major advantages over SPME for most of these aspects. [ABSTRACT FROM AUTHOR]

For measurement of biomarkers from polycyclic aromatic hydrocarbon (PAH) exposure, an analytical method is described quantifying hydroxylated PAH (OH-PAH) in urine samples. This method determined monohydroxy metabolites of naphthalene, fluorene, phenanthrene, fluoranthene, pyrene, chrysene, benzo[ c]phenanthrene, and benz[ a]anthracene. The sample preparation consisted of enzymatic hydrolysis, solid-phase extraction and derivatization with a silylating reagent. Five carbon-13 labeled standards were used for isotope dilution. Analytes were separated by gas chromatography (GC) and quantified with high-resolution mass spectrometry (HRMS). This method produced good recoveries (41–70%), linearity, and specificity. Data were corrected for blank levels from the naphthalene, fluorene, and phenanthrene metabolites. Method detection limits ranged from 2 ng L–1 for 1-hydroxypyrene to 43.5 ng L–1 for 1-hydroxynaphthalene. Using quality control charts from two urine pools, the method can be readily applied to biomonitoring PAH exposure. [ABSTRACT FROM AUTHOR]