采用高效液相色谱-串联质谱法测定血中欧夹竹桃苷和欧夹竹桃苷乙的含量。血液样品在固相支撑液液萃取柱上分散及固定后，用乙酸乙酯进行洗脱。所得洗脱液用于色谱分离，以Kinetex C₁₈色谱柱为分离柱，以不同体积比的含0.1%（体积分数）甲酸的10 mmol·L^-1甲酸铵溶液和乙腈所组成的混合液为流动相进行梯度洗脱。在串联质谱分析中，采用电喷雾正离子源多反应监测模式检测。欧夹竹桃苷和欧夹竹桃苷乙的质量浓度均在2~100 μg·L^-1内与其峰面积呈线性关系，方法的检出限（3S/N）均为0.5 μg·L^-1。以空白样品为基体进行加标回收试验，所得回收率在90.0%~98.0%之间，测定值的相对标准偏差（n=6）在2.1%~7.3%之间。

HPLC-MS/MS was applied to the determination of oleandrin and adynerin in blood. The blood sample was dispersed and affixed on solid phase supported liquid-liquid extraction column which was then eluted with ethyl acetate. The eluate was then separated by using Kinetex C₁₈ chromatographic column as stationary phase, and mixtures of 10 mmol·L^-1 ammonium formate solution[containing 0.1% (φ) formic acid] and acetonitrile in various ratios as mobile phase in gradient elution. ESI⁺ and multi-reactions monitoring were adopted in MS/MS. Linear relationships between values of peak area and mass concentration of oleandrin and adynerin were kept in the same range of 2-100 μg·L^-1, with same detection limit (3S/N) of 0.5 μg·L^-1. On the base of blank sample, test for recovery was made by standard addition method; values of recovery found were in the range of 90.0%-98.0%, with RSD's (n=6) in the range of 2.1%-7.3%.