Solid-phase extraction and derivatisation methods for beta-blockers in human post mortem whole blood, urine and...

This paper details various rapid and sensitive methods for the extraction and derivatisation of propranolol, metoprolol, sotalol, atenolol, pindolol, timolol, oxprenolol, alprenolol and penbutolol in equine urine and in human post mortem whole blood and urine. Three solid-phase extraction methods are described involving the use of either XtrackT XRDAH515, Bond Elut Certify or Sep-Pak C18 cartridges. Two derivatisation methods are also described involving the formation of cyclised silyl or pentafluoropropionate derivatives with either chloromethyldimethylchlorosilane or pentafluoropropionic anhydride, respectively. Gas chromatographic-mass spectrometry analysis was carried out in select-ion monitoring mode. All these methods were evaluated using drug-free human post mortem blood, urine and equine urine fortified at various levels with the beta-blockers mentioned above. The application of some of these methods on a forensic case study is also presented. This work does not include samples from equine administration trials of beta-blockers.