雏菊叶龙胆酮快速制备与标准化分析

Rapid preparation and standardization analysis of Bellidifolin

以龙胆科獐牙菜属植物抱茎獐牙菜(Swertia franchetiana H.Smith)全草为原料,建立了基于制备液相色谱技术的雏菊叶龙胆酮快速制备工艺,从500 g抱茎獐牙菜中分离获得1.66 g雏菊叶龙胆酮样品,之后完成纯度分析、结构鉴定、均匀性检查、稳定性检验和定值标准化分析研究。基于HPLC技术,采用不同的检测波长进行纯度测试,纯度均大于98%;基于LC-MS对制备的样品进行纯度测试,未发现明显杂质峰存在;经1H-NM R和13C-NM R确定其结构为1,5,8-三羟基-3-甲氧基山酮(雏菊叶龙胆酮)。该样品均匀性良好,4℃条件下24个月内稳定性良好,定值结果确定其纯度为99.57%,在95%置信区间范围内的相对扩展不确定度为0.50%。

A rapid preparation process of Bellidifolin from whole herb of Swertia franchetiana H.Smith was established by prep-HPLC.As a result,1.66 g of Bellidifolin was obtained from 500 g of the whole plant.Afterwards,purity analysis,structure identification,homogeneity and stability inspection,and cooperative certification were conducted.HPLC analysis showed the purity of the prepared sample was higher than 98%with no obvious impurity peaks by using different detection wavelengths.The structure was determined as 1,5,8-trihydroxy-3-methoxyxanthone(Bellidifolin)by 1H-NMR and 13C-NMR.The results indicated that the homogeneity of Bellidifolin was excellent,with good stability within 24 months at 4℃.The certified value of the reference material of Bellidifolin was 99.57%with the expanded uncertainty of 0.50%in confidence coefficient of 95%.