A highly sensitive liquid chromatography-tandem mass spectrometry method was developed and validated for the determination of typhaneoside in rat plasma using rutin as internal standard. The analyte and rutin (internal standard) were extracted with methanol followed by a rapid isocratic elution with 10 mM ammonium acetate buffer/methanol (v:v, 20:80) on an C(18) column (150 mm × 2.1 mm I.D.) and subsequent analysis by mass spectrometry in the multi-reaction-monitoring mode. The precursor to product ion transitions of m/z 769.3 → 314.1 and m/z 609.2 → 300.1 were used to measure the analyte and the internal standard. The assay was linear over the concentration range of 0.01-10 μg/mL for typhaneoside in rat plasma. The lower limit of quantification was 0.01 μg/mL and the extraction recovery was larger than 90.2% for typhaneoside. The inter- and intra-day precision of the method at three concentrations was less than 6.8%. The method was firstly applied to pharmacokinetic study of typhaneoside in rats.
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