A method was developed for the determination of amygdalin and its metabolite pru-nasin in rat plasma after intragastric administration of Maxing shigan decoction. The analytes were identified by ultra-high performance liquid chromatography-tandem quadrupole time of flight mass spectrometry and quantitatively determined by ultra-high performance liquid chroma-tography-tandem triple quadrupole mass spectrometry. After purified by liquid-liquid extraction, the qualitative analysis of amygdalin and prunasin in the plasma sample was performed on a Shim-pack XR-ODS Ⅲ HPLC column( 75 mm × 2. 0 mm,1. 6 μm ),using acetonitrile-0. 1%( v / v)formic acid aqueous solution. The detection was performed on a Triple TOF 5600 quadru-pole time of flight mass spectrometer. The quantitative analysis of amygdalin and prunasin in the plasma sample was performed by separation on an Agilent C 18 HPLC column(50 mm ×2. 1 mm,1. 7 μm),using acetonitrile-0. 1%(v / v)formic acid aqueous solution. The detection was performed on an AB Q-TRAP 4500 triple quadrupole mass spectrometer utilizing electrospray ionization( ESI) interface operated in negative ion mode and multiple-reaction monitoring (MRM)mode. The qualitative analysis results showed that amygdalin and its metabolite pruna-sin were detected in the plasma sample. The quantitative analysis results showed that the linear range of amygdalin was 1. 05 - 4 200 ng / mL with the correlation coefficient of 0. 999 0 and the linear range of prunasin was 1. 25-2 490 ng / mL with the correlation coefficient of 0. 997 0. The method had a good precision with the relative standard deviations( RSDs)lower than 9. 20%and the overall recoveries varied from 82. 33% to 95. 25% . The limits of detection( LODs)of amygdalin and prunasin were 0. 50 ng / mL. With good reproducibility,the method is simple,fast and effective for the qualitative and quantitative analysis of the amygdalin and prunasin in plas-ma sample of rats which were administered by Maxing shigan decoction.%建立了大鼠灌胃麻杏石甘汤后血浆中苦杏仁苷、野黑樱苷的定性及定量方法。样品经液液萃取净化处理，定性采用超高效液相色谱-串联四极杆飞行时间质谱仪（UPLC-QTOF-MS / MS），经 Shim-pack XR-ODS Ⅲ色谱柱（75 mm×2.0 mm，1.6μm）分离，定量采用超高效液相色谱-串联三重四极杆质谱仪（ UPLC-Q-TRAP-MS），经 Agilent C18色谱柱（50 mm×2.1 mm，1.7μm）分离，电喷雾负离子化（ ESI）及 MRM 模式测定，流动相均为乙腈-0.1％（ v /v）甲酸水溶液。结果显示苦杏仁苷、野黑樱苷在相应浓度范围内线性关系良好（相关系数分别为0.9990、0.9970），精密度（RSD）小于9.20％，回收率为82.33％~95.25％，检出限（ LOD）约为0.50 ng / mL。本方法快速简便，为血浆样品中苦杏仁苷、野黑樱苷的定性和定量分析提供良好参考。
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