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A liquid chromatographic method using a solid-phase extraction procedure for the quantification of sotalol in plasma and urine is described. Sotalol is eluted from an extraction column with ethyl acetate-acetonitrile (1:2) and, after separation by reversed-phase high-performance liquid chromatography on a mu Bondapak C18 column, is quantified by fluorescence detection at excitation and emission wavelengths of 240 and 310 nm, respectively. The method has been demonstrated to be linear over the concentration ranges 10-6000 ng/ml in plasma and 0.5-100 micrograms/ml in urine. Mean inter-assay accuracy of the method for plasma ranged from 93 to 100% and for urine from 102 to 114%; precision ranged from 0.5 to 1.6% for plasma over a concentration range of 200-4000 ng/ml and for urine from 0.7 to 2.0% at concentrations of 2-50 micrograms/ml. Mass spectrometry confirmed the presence of sotalol in isolated chromatographic fractions of plasma and urine extracts from subjects given sotalol orally.

A method for determining bucindolol, a deuterated analogue and two metabolites in plasma samples is described. Analytes are obtained from plasma by liquid extraction of 1 ml of plasma at pH 10.5 with 7 ml of peroxide-free ether-hexane (4:1). Following derivatization with 50 microliters of N-methyl-N-trimethylsilyl trifluoroacetamide-pyridine (1:1) for 20 min at 65 degrees C the samples are analyzed by capillary column gas chromatography-mass spectrometry with selected-ion monitoring. Quantification is linear over the range 2-500 ng/ml. Single-day precision was typically 6.2% or better for bucindolol and 13% or better for the metabolites.