大麦黄苷和皂草黄苷标准样品的制备与标准化研究

Research of preparation and standardization of lutonarin and saponarin standard samples

以禾本科植物大麦的幼苗为原料,建立了基于制备型高速逆流色谱技术的大麦黄苷和皂草黄苷标准样品的规模化快速制备工艺,从200 g大麦幼苗中制得1.2 g大麦黄苷和1.6 g皂草黄苷。经HPLC和HPLC/MS分析,纯度均大于99%,无明显杂质峰;经1H-NMR和13C-NMR确定其结构为大麦黄苷和皂草黄苷。该样品在95%置信区间均匀性良好,4℃条件下24个月内稳定性良好,定值结果确定其纯度分别为99.59%和99.52%,相对扩展不确定度(包含因子k=2)分别为0.52%和0.50%。

Taking the seedlings of Hordeum vulgare L. as raw materials, a rapid and large-scale preparation process for lutonarin and saponarin standard samples based on preparative high-speed countercurrent chromatography was established. 1.2 g of lutonarin and 1.6 g of saponarin were prepared from 200 g of barley seedlings. HPLC and HPLC/MS analysis showed that the purities of lutonarin and saponarin were more than 99%, and no obvious impurity peak was found. The structures were identified as lutonarin and saponarin by 1HNMR and 13C-NMR. The samples have satisfactory uniformity within the 95% confidence interval and favourable stability within 24 months at 4℃. The certificated value was determined as 99.59% and 99.52%, respectively.The relative expanded uncertainty values were 0.52% and 0.50%, respectively, with the coverage factor of 2.