Quantitative determination of tertatolol in biological fluids by gas chromatography-mass spectrometry.

Quantitative determination of tertatolol concentrations in plasma and urine was performed by gas chromatography-mass spectrometry in the chemical-ionization mode with ammonia after successive extractions of the beta-blocking drug in alkaline, acid and final alkaline medium. [2H9]Tertatolol, isotopically stable under the operating conditions employed, was used as an internal standard, thus allowing quantities of 1 ng/ml to be specifically determined. Overall analytical error was less than 10%. Prior to isothermal chromatography at 240 degrees C on a column packed with 3% SE-30, both compounds were silylated with bis(trimethylsilyl)trifluoroacetamide. Detection was performed by monitoring the quasimolecular ions of tertatolol, m/z 368 and m/z 377, for the [2H9]tertatolol in the chemical-ionization mode with ammonia. The calibration curves obtained had linear characteristics for the concentration range 1-1125 ng/ml.