藏药诃子质量标志物诃黎勒酸的标准化分析研究  

Standardization of Chebulagic Acid as Quality Marker of Tibetan Medicine Terminalia Chebula

作　　者：宋志博 陈涛[1,5] 王肖波 王岱杰 申诚[1] 王硕 李洪梅[1,5] 海平[4] 李玉林 SONG Zhibo;CHEN Tao;WANG Xiaobo;WANG Daijie;SHEN Cheng;WANG Shuo;LI Hongmei;HAI Ping;LI Yulin(Northwest Institute of Plateau Biology,Chinese Academy of Sciences,Xining 810001,China;Northwest Institute of Eco-Environment and Resources,Chinese Academy of Sciences,Lanzhou 730000,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 and Tibentan Medicine,Xining 810016,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]中国科学院西北生态环境资源研究院,甘肃兰州730000 [3]山东省分析测试中心,山东济南250014 [4]青海省药品检验检测院国家药品监督管理局中药(藏药)质量控制重点实验室,青海西宁810016 [5]中国科学院大学,北京100049

出　　处：《分析测试技术与仪器》2023年第2期140-148,共9页Analysis and Testing Technology and Instruments

基　　金：青海省重点研发与转化计划:藏药质量标志物发掘和标准化关键技术及应用示范(2023-SF-112),甘肃省青年科技基金计划(20JR5RA542)。

摘　　要：以藏药诃子为原料,研制诃黎勒酸国家标准样品.诃子经60%乙醇提取,大孔树脂富集,制备液相色谱技术得到诃黎勒酸标准品.采用高效液相色谱(HPLC)、液相色谱-质谱(LC-MS)和薄层色谱(TLC)等手段进行纯度分析.采用紫外光谱(UV)、红外光谱(IR)、高分辨质谱(MS)和核磁共振波谱(NMR)技术进行结构确认.最后进行均匀性、稳定性和联合定值.结果表明,诃黎勒酸样品均匀性良好,4℃储存,24个月内稳定.联合定值确定诃黎勒酸纯度标准值为99.33%,符合国家标准品的要求.研制出的诃黎勒酸(GSB11-3724-2020)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 of chebulagic acid has been developed using a Tibetan medicine Terminalia Chebula as the raw material.Terminalia Chebula was extracted with 60%ethanol,enriched by the macroporous resin and through the preparative liquid chromatographic purification to obtain chebulagic acid.The purity analysis was carried out by high performance liquid chromatography(HPLC),liquid chromatography-mass spectrometry(LC-MS)and thin-layer chromatography(TLC).The structure was identified using ultraviolet(UV)spectroscopy,infrared(IR)spectroscopy,mass spectroscopy(MS)and nuclear magnetic resonance(NMR)spectroscopy.Finally,the homogeneity,stability and cooperative certification were carried out.The results indicated that the chebulagic acid has a good uniformity and a fine stability within 24 months at 4℃.The standard value of the purity of chebulagic acid was 99.33%,which was in accordance with the requirements of the certified reference material.The developed chebulagic acid(GSB 11-3724-2020)can be used for the content determination,method evaluation,testing and quality control of related products.

关 键 词：诃黎勒酸 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]