山东科学 ›› 2016, Vol. 29 ›› Issue (1): 14-20.doi: 10.3976/j.issn.1002-4026.2016.01.003

• 中药与天然活性产物 • 上一篇    下一篇

松果菊苷标准样品的研制

王婷婷1,赵敏1,王岱杰2,郑媛媛3,任汉书3,耿岩玲2*   

  1. 1山东农业工程学院,山东 济南 251100; 2 山东省中药质量控制技术重点实验室,山东省分析测试中心,山东 济南 250014; 3 广饶县中医院,山东 东营 370523
  • 收稿日期:2015-07-22 出版日期:2016-02-20 发布日期:2016-02-20
  • 通信作者: 耿岩玲(1973-),女,副研究员,研究方向为天然产物提取分离及标准样品制备。 E-mail:gengyanling@126.com
  • 作者简介:王婷婷(1986-),女,硕士,研究方向为食品质量与安全。Email:383766725@qq.com
  • 基金资助:

    2013国家质检公益性行业科研专项(201310243); 山东省科技发展计划(2014GZX219003)

Preparation of the certified reference material of Echinacoside

WANG Tingting1, ZHAO Min1,WANG Daijie2, ZHENG Yuanyuan3,REN Hanshu3, GENG Yanling2*   

  1. 1.Shandong Agriculture and Engineering University,Jinan 251100, China; 2. Shandong Provincial Key Laboratory of TCM Quality Control Technology, Shandong Analysis and Test Center, Jinan 250014, China; 3. Guangrao County Traditional  Chinese Medicine Hospital, Dongying 370523, China
     Chinese Medicine Hospital, Dongying 370523, China
  • Received:2015-07-22 Online:2016-02-20 Published:2016-02-20

摘要:

建立了松果菊苷标准样品的研制方法。采用柱色谱和高速逆流色谱联用对松果菊苷进行分离制备,采用质谱、紫外、红外和核磁等方法对松果菊苷进行结构表征,并进行均匀性和稳定性检验。经国内8个有资质的实验室联合定值,松果菊苷标准样品的标准值为9915%,不确定度值为066%(置信度95%),达到国家标准样品的技术要求,可用于松果菊苷检测和相关产品的分析测试和质量控制。

关键词: 松果菊苷, 标准样品, 均匀性, 稳定性, 定值

Abstract:

We presented preparation technique of the certified reference material for Echinacoside. We employed column chromatography and highspeed countercurrent chromatography to separate and prepare Echinacoside, and MS, UV, IR and NMR to elucidate its chemical structure. We also checked its homogeneity and stability. It was then cooperatively certified through eight domestic qualified laboratories. Results show that it has certified value of 99.15%, expanded uncertainty of 0.66% (corresponding to confidence coefficient of 95%). This demonstrates that it conforms with technical requirements on a certified reference material, so it can be applied to Echinacoside detection and analysis and test and quality control of relative products.

Key words: certified reference material, certification, homogeneity, stability, Echinacoside

中图分类号: 

  • R284.1