厚朴中和厚朴酚标准样品的研制

Preparation of Certified Reference Materials of Honokiol from M. officinalis

依据GB/T 15000.3-2008标准样品的工作导则,研制和厚朴酚标样样品。以厚朴药材的提取物为原料,采用高速逆流色谱法一步分离制备和厚朴酚单体化合物,通过紫外光谱、红外光谱、质谱、1H和13C核磁共振等技术手段进行化合物的结构表征,同时进行了薄层色谱、液质联用和热重分析纯度和水分含量,建立了和厚朴的高效液相色谱分析检测技术。和厚朴酚样品进行了均匀性检验、稳定性检验和8家实验室联合定值。结果表明,和厚朴酚样品具有良好的均匀性,在0~4℃储存条件下48个月含量稳定。将定值结果分析统计,确定其标准值为99.72%,置信度95%的不确定度为0.22%。成功研制出了和厚朴酚国家标准样品,达到了GB/T15000.3-2008规定的技术要求,样品具有溯源性,可用于和厚朴酚及相关产品的质量控制和检测方法评定。

The certified reference material（CRM） of honokiol was develpoed according to the technical requirements of CRM General and Statistical Principle for Certification（GB/T 15000.3-2008）. Honokiol was separated and prepared by high-speed counter-current chromatography with crude extracts of Magnolia officinalis Rehd. et Wils. as material, and their structures were confirmed by UV, IR, MS, 1 H and 13 C NMR. Simultaneously, the purity and moisture content of Honokiol was analyzed by thin layer chromatography, LC-MS, and thermo-gravimetric to establish HPLC analysis technology. Honokiol was divided into bottles for homogeneity test, stability test, and cooperative certification by 8 laboratories. The results indicated that the homogeneity of honokiol samples were excellent, with good stability within 48 months at 0-4oC. The certified value of the reference material of honokiol was 99.72% with the expanded uncertainty of 0.22% in confidence coefficient of 95%. The reference material of honokiol was successfully developed, which reached the technical requirement of GB/T 15000.3-2008 and could be traceable. The CRM can be used in the content determination and testing method validation of honokiol related products.