Comparison of Sample Preparation and Analysis Using Solid-Phase Extraction and Solid-Phase Microextraction to Determine Monohydroxy PAH in Urine by GC/HRMS

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.