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A liquid chromatography−mass spectrometry method was developed for the simultaneous quantitation of (2R,3R)-Dihydromyricetin and Myricetin in rat plasma samples to facilitate analysis of samples collected after administration of SenDeng-4 medicine. The plasma was subjected to protein precipitation with HCl (containing 10% ascorbic acid) and analyzed using electrospray ionization mass spectrometry in selected ion monitoring mode with Paeoniflorin as an internal standard. Good linearity for the two compounds was observed. The intra- and inter-day precision of analysis was <10% for each compound. The present method was suitable for determining (2R,3R)-Dihydromyricetin and Myricetin in rat plasma after intravenous administration of SenDeng-4 to rats with sufficient sensitivity. [ABSTRACT FROM AUTHOR]