Abstract
The most convenient way to perform supercritical fluid extraction (SPE) of liquid sample matrices is to combine it with solid-phase extraction (SPE). β-Blockers from urine were collected on an Empore disc, which was then placed into an extraction cell for derivatization and SPE. SPE recovery was best at pH 10. Effects of temperature, pressure and volume of pyridine on the acetylation and SFE processes were studied. Without acetylation the β-blockers were not significantly soluble in CO 2. SFE temperatures of 70°C and 150°C together with 200 μl of acetic anhydride and 400 μl pyridine gave the best results. With the SPE-SFE-GC-MS method developed here, β-blockers like oxprenolol, metoprolol and propranolol could easily be detected in urine samples, and the limit of detection (LOD) for these compounds was found to be 20 ng/ml, 30 ng/ml and 40 ng/ml, respectively.
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