白鲜皮中黄柏酮标准样品的研制

Preparation of certified reference materials of obacunone from bark of Dictamnus dasycarpus Turcz

依据GB/T 15000.3-2008标准样品的工作导则,研制黄柏酮标准样品。以白鲜皮为原料,硅胶柱色谱结合重结晶的方法制备黄柏酮单体,通过UV、IR、MS和NMR等技术进行结构表征,同时进行了薄层色谱鉴别和热重分析,通过HPLC检测分析技术,进行了均匀性检验、稳定性检验和8家实验室联合定值。结果表明,该样品均匀性良好,在0~4℃储存24个月稳定性良好,定值结果确定其标准值为98.94%,置信度95%的不确定度为0.12%。说明,黄柏酮标准样品达到了GB/T 15000.3-2008规定的技术要求,具有溯源性,可用于黄柏酮及相关产品的质量控制和检测方法评定。

The certified reference material（ CRM） of obacunone was researched according to the technical requirement of general and statistical principle for certification GB/T 15000.3-2008. Using bark of Dictamnus dasycarpus Turcz as material,the obacunone sample was obtained by the method of silica gel chromatography combined with the recrystallization,and the structure was identified by UV,IR,MS and NMR. The purity of obacunone was analyzed by thin-layer chromatography,thermogravimetric and HPLC technology. The samples were investigated by homogeneity test,stability test,and cooperative certification performed by eight laboratories. The results indicated that the obacunone sample had good homogeneity and good stability after storage at 0-4 ℃ for 24 months. The certified value of of obacunone was 98.94% with a expanded uncertainty of 0.12% in confidence level of 95%. The reference material of obacunone was conformed to the technical requirement of GB/T 15000.3-2008 and could be traceable. So,the CRM of obacunone could be used for quality control and test method evaluation of obacunone and related products.