肉桂醛标准样品的研制  

Development of Certified Reference Material of Cinnamaldehyde

作　　者：马玉翠[1] 吴翠[1] 王尉[2] 王淳[1] 杜宁[2] 王金[1] 吴晓毅[1] 巢志茂[1] 

机构地区：[1]中国中医科学院中药研究所,北京100700 [2]北京市理化分析测试中心,北京100094

出　　处：《中国实验方剂学杂志》2017年第8期67-71,共5页Chinese Journal of Experimental Traditional Medical Formulae

基　　金：国家质量监督检验检疫总局行业科研专项(201210209);国家标准化管理委员会国家标准样品研制项目(S2012090)

摘　　要：目的:依据GB/T 15000.3-2008《标准样品工作导则(3)标准样品:定值的一般原则和统计方法》,在国家标准化管理委员会批准立项的基础上,研制肉桂醛国家标准样品。方法:以樟科植物肉桂的干燥树皮为原料,通过提取,NaHSO_3加成反应,制备高效液相色谱,纯化得到了肉桂醛样品,采用元素分析,UV,IR,MS和NMR进行了结构鉴定。进行了薄层色谱的鉴别。建立了高效液相色谱紫外检测分析技术。样品分装成200瓶(每瓶20 mg)样品后,进行了均匀性检验、稳定性检验和8家实验室的联合定值。结果:该样品均匀性良好,0~8℃条件下,24个月内稳定性良好,定值结果为98.41%,95%置信区间的扩展不确定度为0.06%,达到了国家标准样品的技术要求,通过了国家标准化管理委员会组织的验收。结论:成功地研制了肉桂醛国家标准样品,可用于肉桂醛含量测定、检测方法评定、相关产品的检测与质量控制。Objective： To develop a certified reference material （CRM） of cinnamaldehyde according to The Directives for the Work of Reference Materials （3）： Reference Material-General and Statistical Principles for Certification （GB/T 15000.3-2008） based on the CRM project approved by Standardization Administration of the People＇s Republic of China （SAC）. Method： Cinnamaldehyde was obtained by means of extraction, NaHSO3 additive reaction, and preparative high performance liquid chromatography from the dried Cinnamomi Cortex. The structure of cinnamaldehyde was confirmed by element analysis, UV, IR, HRMS, NMR. Thin layer chromatography was carried out for the identification. The sample of cinnamaldehyde was divided into 200 bottles with 20 mg per bottle. The homogeneity test, stability test, and quantitative analysis were carried out by high performance liquid chromatography with an ultra violet detector. Result： The homogeneity of CRM of cinnamaldehyde was excellent, and the storage period for cinnamaldehyde was 24 months at 0-8℃. The certified purity value of the CRM of cinnamaldehyde was 98.41% with an expand uncertainty of 0.06%. This CRM corresponded with the technical requirement of a series of GB/T 15000.3 guides about the CRM and was checked and accepted by SAC. Conclusion： The national CRM of cinnamaldehyde was developed for the first time. This CRM is intended for use in the method validation, testing, and quality control regarding cinnamaldehyde.

关 键 词：肉桂醛 标准样品 均匀性 稳定性 定值 不确定度 

分 类 号：R284.1[医药卫生—中药学]