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| - Direct Plasma Analysis of Drug Compounds UsingMonolithic Column Liquid Chromatography andTandem Mass Spectrometry
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| - A monolithic silica column high-performance liquid chromatography−tandem mass spectrometry (HPLC−MS/MS)method has been developed for the high-speed directsimultaneous determination of a drug discovery compound and its major circulating metabolite (M-72) in ratplasma. This methodology makes use of flow programming and an alkyl-bonded silica rod column for fastmacromolecule removal and chromatographic separationwithout the need for significant sample preparation. Thematrix ionization suppression effect on the monolithiccolumn HPLC−MS/MS system was investigated using thepostcolumn infusion technique. After 200 plasma injections on a 50 × 4.6 mm monolithic silica column,consistent column efficiency of close to 39 000 theoreticalplates/m and reproducible retention times for the analyteswere observed. The apparent on-column recoveries of 12test compounds in rat plasma samples were greater than90%. The proposed fast direct plasma injection methodwas tested over a 3-day period with the interday coefficientof variation less than 15% for both analytes.
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