酸枣仁总黄酮和总皂苷部位制备工艺的稳定性考察

Stability of Preparation Process of Total Flavonoids and Total Saponins from Ziziphi Spinosae Semen

目的：考察酸枣仁总黄酮和总皂苷部位制备工艺的稳定性,为后续药效学评价的样品制备提供保证。方法：采用相同工艺条件制备10批酸枣仁总黄酮和总皂苷部位样品。选择斯皮诺素、白桦酯酸及酸枣仁皂苷A,B为指标成分,利用ELSD/HPLC分析两部位样品的特征图谱,流动相乙腈（A）-水（B）梯度洗脱（0~10 min,12%~18%A;11~20 min,19%~23%A;21~30 min,23%~34%A;31~40 min,35%~45%A;41~50 min,46%~100%A;51~60 min,100%~11%A;61~70 min,12%A）,漂移管温度40℃。结果：总黄酮部分的化学成分分布主要集中于前25 min,总皂苷部分化学成分集中在25 min后,总黄酮和总皂苷纯度均〉50%,54.46 min处色谱峰确定为白桦酯酸。结论：制备酸枣仁总黄酮和总皂苷部位的工艺稳定性良好,可作为药效学试验的样品。

Objective： Stability of preparation process of total flavonoids and total saponins from Ziziphi Spinosae Semen was investigated, in order to provide a guarantee for sample preparation of follow- pharmacodynamie evaluation. Method： Ten batches of total flavonoids and total saponins from Ziziphi Spinosae Semen were prepared with the same preparation process. Spinosin, betulinie acid, jujuboside A and jujuboside B were taken as index components, ELSD/HPLC was employed to analyze feature profiles of these two parts samples with mobile phase of acetonitrile （A） -water （B） for gradient elution （0-10 rain, 12% -18% A; 11-20 min, 19%-23%A; 21-30 min, 23%-34% A; 31-40 min, 35%-45% A; 41-50 rain, 46%-100% A; 51-60 min, 100%-11%A; 61-70 min, 12% A） and drift tube temperature of 40 ~C. Result： Chemical compositions distribution of total flavonoids part focused on the fomer 25 min, but that of total saponins concentrated in after 25 min,purities of total flavonoids and total saponins were more than 50% , peak at 54.46 rain was identified as betulinic acid. Conclusion ： This preparation technology of total flavonoids and total saponins from Ziziphi Spinosae Semen is stable, which can be used as samples of pharmacodynamie experiment.