宝藿苷Ⅰ纯度标准物质的研制
孙欣光1,黄文华1,郭宝林1,丁晓静2,贺圆1,刘军3
中国医学科学院北京协和医学院药用植物研究所,中草药物质基础与资源利用教育部重点实验室,北京 100193;北京市疾病预防控制中心,北京 100013;中国计量科学研究院化学计量与分析科学研究所,北京 100013
Development of Baohuoside Ⅰ Purity Certified Reference Material
孙欣光1,黄文华1,郭宝林1,丁晓静2,贺圆1,刘军3
1. The Key Laboratory of Bioactive Substances and Resources Utilization of Chinese Herbal Medicine, Ministry of Education, Institute of Medicinal Plant Development, Chinese Academy of Medical Sciences & Peking Union Medical College, Beijing 100193, China; 2. Beijing Center for Disease Control and Prevention, Beijing 100013, China; 3. Division of Metrology in Chemistry, National Institute of Metrology, Beijing 100013, China
摘要:以淫羊藿提取物为原料,通过正相硅胶柱色谱和凝胶柱色谱等分离纯化手段,研制了宝藿苷 Ι 纯度标准物质。采用液相色谱 -质谱法和核磁共振技术对宝藿苷Ⅰ纯度标准物质进行定性鉴定,利用高效液相色谱(HPLC)法和胶束电动毛细管色谱(MECC)法对宝藿苷 Ι 的纯度进行定值分析,同时利用 HPLC 法对宝藿苷 Ι 纯度标准物质进行均匀性检验与稳定性考察,通过 F 检验和 t 检验法对其均匀性进行检验,表明瓶间和瓶内均匀性一致,12 个月稳定性检验结果的相对标准偏差为 0.02%,说明宝藿苷 Ι 纯度标准物质是稳定的。对定值结果的不确定度进行了评价,研制的宝藿苷 Ι 纯度标准物质的定值结果和扩展不确定度分别为 99.7% 和 0.3%(k=2)。
Abstract:Baohuoside Ⅰ was extracted from the leaves of epimedium brevicornu maxim, the extract was isolated by silica gel column chromatography and was purified further over Sephadex LH-20 column chromatography, and Baohuoside Ⅰ purity certified reference material (CRM) was presented. The qualitative analysis of Baohuoside Ⅰ purity CRM material was performed by high performance liquid chromatography-mass spectrometry(HPLC-MS) and nuclear magnetic resonance(NMR). The purity of BaohuosideⅠ was determined by high performance liquid chromatography (HPLC) and micellar electrokinetic capillary chromatography (MECC). Homogeneity and stability monitoring of BaohuosideⅠ purity CRM were performed by HPLC. Homogeneity was evaluated by F-test and t-test, the stability was monitored over 12 month, and the RSD of stability was 0.02%. The uncertainty evaluation was studied extensively. The certified purity value of Baohuoside Ⅰ purity CRM was 99.7% with expanded uncertainty of 0.3 %(k=2).
关键词:宝藿苷Ι纯度标准物质;制备;高效液相色谱法;胶束电动毛细管色谱法;不确定度评定
Keywords:BaohuosideⅠ purity CRM; development; high performance liquid chromatography; micellar electrokinetic capillary chromatography; uncertainty evaluation
基金:国家科技支撑计划(21-09-4GZ-13)
本文引用格式:
孙欣光,黄文华,郭宝林,等.GC-MS校准用异辛烷中八氟萘标准溶液的研制[J].化学分析计量,2014,23(2):1-5.
相似文章: