High-throughput monospin extraction for quantification of cardiovascular drugs in serum coupled to high-performance liquid chromatography–mass spectrometry

A novel method coupling spin column extraction with high-performance liquid chromatography–mass spectrometry was developed for simultaneous extraction of β-blockers and calcium channel blockers from human serum. Sample loading, washing, and elution were accomplished via centrifugation of the column, in which mixed-mode monolithic silica bonded to a C18 reversed phase, and a cation-exchange phase was packed in a spin column. The serum sample (0.2 mL) pH was adjusted to 3 and the analytes adsorbed onto the column were eluted with 0.1 mL MeOH containing 2% NH3. The recoveries of the tested drugs were 76–108%. A linear curve was observed up to a concentration of 500 ng/mL of the target drugs in serum (r2 > 0.996). The intra-day relative standard deviations at three different concentrations were 0.6–9.6%. The limits of detection were 2 ng/mL. The proposed method was successfully applied to clinical and forensic cases.