白鲜中梣酮标准样品的制备

Study on the Preparation of Fraxinellone Standard Sample from Dictamnus dasycarpus

目的:制备梣酮标准样品,确保梣酮及相关产品检测的准确性、可比性和可溯源性。方法:以芸香科植物白鲜的干燥根皮为原料,采用硅胶柱色谱分离制备梣酮单体。分别采用高效液相色谱(HPLC)法、薄层色谱(TLC)法和液质联用(LC-MS)技术对梣酮单体纯度进行分析,通过紫外光谱、红外光谱、质谱和核磁共振等波谱技术对梣酮单体的结构进行表征,并参照GB/T 15000.3标准样品的工作导则要求考察其均匀性、稳定性和定值。结果:HPLC、TLC和LC-MS检测结果显示,所制单体纯度较高,在相关图谱中无明显杂质峰或斑点存在;经多种波谱技术鉴定分离单体化合物为梣酮;所制梣酮单体的均匀性良好,10瓶样品间纯度差异无统计学意义(P>0.05);梣酮单体在0~4℃条件下贮藏24个月稳定性良好,稳定性的扩展不确定度为0.16%;8家实验室联合定值试验确定其标准值为99.75%,扩展不确定度为0.34%。结论:成功制备了符合GB/T 15000.3要求的梣酮标准样品,该样品可用于梣酮及相关产品的质量控制和检测方法的评定。

OBJECTIVE：To prepare fraxinellone standard sample,and guarantee accuracy,comparability and traceability of fraxinellone and related products. METHODS：Fraxinellone monomer was obtained by means of silica gel chromatography from dried bark of Dictamnus dasycarpus. HPLC,TLC and LC-MS were used to analyze the purity of fraxinellone monomer. Their structures were confirmed by UV,IR,MS and NMR. Homogeneity,stability and constant value of it were investigated by referring to GB/T 15000.3 standard sample. RESULTS：Results of HPLC,TLC and LC-MS showed that the purity of prepared monomer was high. No significant impurity peak or spot was found in related chromatograms. A variety of spectroscopic techniques were used to identify prepared monomeric compound as fraxinellone. Prepared fraxinellone monomer had good uniformity, there was no statistical significance in purity difference among 10 samples（P〉0.05）. The stability of prepared fraxinellone monomer was good at0-4 ℃ for 24 months,the extended uncertainty of stability was 0.16%. The standard value of fraxinellone monomer was 99.75% in combination constant value tests of 8 laboratories,and expanded uncertainty was 0.34%. CONCLUSIONS：The fraxinellone was successfully prepared that was conformed to the technical requirement of GB/T 15000.3,and it can be used in the content determination and testing method validation of fraxinellone related products.