藏药诃子质量标志物诃子酸的分离分析及标准化研究  

Separation and Standardization of Chebulinic Acid as Quality Marker of Tibetan Medicine Terminalia Chebula

作　　者：宋志博 陈涛[1,5] 王岱杰 邹登朗[4] 王硕 李洪梅[1,5] 刘亚蓉[3] 杨凤梅 海平 李玉林 SONG Zhi-bo;CHEN Tao;WANG Dai-jie;ZOU Deng-lang;WANG Shuo;LI Hong-mei;LIU Ya-rong;YANG Feng-mei;HAI Ping;LI Yu-lin(Northwest Institute of Plateau Biology,Chinese Academy of Sciences,Xining 810001,China;Shandong Analysis and Test Center,Jinan 250014,China;Qinghai Provincial Drug Inspection and Testing Institute,NMPA Key Laboratory for Quality Control of Traditional Chinese Medicine,Tibentan Medicine,Qinghai Provincial Key Laboratory for the study of the Modernization of Tibetan Medicine,Xining 810016,China;Qinghai Normal University,Xining 810008,China;University of Chinese Academy of Sciences,Beijing 100049,China)

机构地区：[1]中国科学院西北高原生物研究所,青海西宁810001 [2]山东省分析测试中心,山东济南250014 [3]青海省药品检验检测院中药(藏药)质量控制重点实验室,青海省中药(藏药)现代化研究重点实验室,青海西宁810016 [4]青海师范大学,青海西宁810008 [5]中国科学院大学,北京100049

出　　处：《分析测试技术与仪器》2021年第3期165-173,共9页Analysis and Testing Technology and Instruments

基　　金：青海省藏药国家标准样品研制科技基础条件平台建设项目(2020-ZJ-T02)。

摘　　要：依据GB/T 15000—2008《标准样品工作导则》的要求,研制诃子酸国家标准样品.以诃子的干燥成熟果实为原料,采用大孔吸附树脂、制备型高效液相色谱技术对标准样品进行制备,经过纯度分析、结构鉴定、均匀性检验、稳定性检验,最后进行联合定值.基于高效液相色谱(HPLC)技术,采用不同检测波长进行纯度测试,样品纯度均大于98%.基于液相-质谱(LC-MS)进行纯度分析,未发现明显杂质峰.通过紫外光谱(UV)、红外光谱(IR)、质谱(MS)、核磁共振(NMR)等技术确定其结构为诃子酸.样品均匀性良好,4℃条件下24个月内稳定性良好.定值结果确定诃子酸纯度为98.08%,在95%置信区间范围内的相对扩展不确定度为0.50%.研制出的诃子酸(GSB 11-3725-2020)国家标准样品可用于含量测定、检测方法评定、相关产品的检测与质量控制.A certified reference material(CRM)of chebulinic acid has been developed according to the technical requirements of GB/T 15000—2008.The CRM of chebulinic acid was obtained using the macroporous adsorption resin and preparative high performance liquid chromatography(HPLC),from the dry ripe fruit of Terminalia chebula.Then,the purity analysis,structure identification,homogeneity and stability inspection,and cooperative certification were conducted.HPLC analysis at different detection wavelengths showed that the purity was more than 98%.Liquid chromatograph-mass spectrometry(LC-MS)analysis showed that no obvious impurity peaks were found.The structure was identified as chebulinic acid by ultraviolet spectroscopy(UV),infrared spectroscopy(IR),mass spectroscopy(MS),nuclear magnetic hydrogen spectroscopy(1 H-NMR)and nuclear magnetic carbon spectroscopy(13 C-NMR).The results indicated that the homogeneity and stability of the CRM were good within 24 months at 4℃.The certified purity value of chebulinic acid was 98.08%.The expanded uncertainty was 0.50% in confidence coefficient of 95%.The CRM of chebulinic acid(GSB 11-3725-2020)can be applied for the content determination,evaluation of detection methods,detection and quality control of related products.

关 键 词：诃子酸 标准样品 均匀性 稳定性 定值 

分 类 号：TQ460.7[化学工程—制药化工]