獐牙菜醇苷国家天然产物标准样品的研制

Research and development of certified reference material of swertioside

以龙胆科獐牙菜属植物川西獐牙菜Swertia mussotii全草为原料,采用醇提,正丁醇萃取,制备型液相色谱法分离,Sephadex LH-20凝胶色谱纯化而得到獐牙菜醇苷样品。用红外、紫外、质谱、核磁进行定性分析,确定结构为7-O-[α-L-吡喃鼠李糖-(1→2)-β-D-吡喃木糖]-1,8-二羟基-3-甲氧基口山酮。进行了均匀性检验、稳定性检验和联合定值,该样品在95%置信区间范围内的均匀性良好,定值结果确定其纯度为98.66%,相对扩展不确定度为0.36%,0~8℃条件下36个月内稳定性良好。天然产物标准样品在天然产物的质量控制中是确认产品质量必不可少的标准参照物,成功研制了獐牙菜醇苷标准样品,通过了国家标准化管理委员会的验收,达到了国家标准样品的技术要求,标准品号GSB 11-3281-2015。獐牙菜醇苷标准样品的成功研制可用于含量测定、检测方法评定、相关产品的检测与质量控制。

The standard sample of natural products is an essential standard reference to determine the quality of the product in the quality control of natural products.To develop a certified reference material(CRM)of swertioside according to the Work Guideline for Reference Materials(3):Reference Material-General Principles and Statistical Method for Certification(GB/T 15000.3-2008),swertioside was purified from whole plant of Swertia mussotii by extraction,isolation and Prep-HPLC to obtain certified reference material of swertioside.The structure of swertioside was identified by IR,UV,high-resolution MS,NMR.Thin layer chromatography,optical rotation,elemental analysis and melting point was carried out for the identification.The purity of the prepared sample was tested from different chromatographic elution conditions,thin layer chromatography and HPLC-MS.Swertioside was divided into 140 bottles,with 10 mg per bottle after homogeneity test,stability test and quantitative analysis.This CRM is 7-O-[α-L-rhamnopyranosyl-(1→2)-β-D-xylopyranosyl];the homogeneity of the 95%confidence interval was good;the certified purity value was 98.66%,with a relative expanded uncertainty of 0.38%;the storage period was 36 months at 0-8℃.Therefore,the CRM of sakuranetin reached the technical requirements of CRM,and was accepted by SAC.Swertioside is successfully developed and can be used for determining content,evaluating test methods,detecting relevant products and controlling quality.