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)。
BaohuosideⅠwas 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 BaohuosideⅠpurity certified reference material（CRM）was presented. The qualitative analysis of BaohuosideⅠpurity CRM material was performed by high performance liquid chromatography-mass spectrometry（HPLC-MS）and nuclear magnetic resonance（NMR）. The purity of Baohuoside Ⅰwas determined by high performance liquid chromatography（HPLC） and micellar electrokinetic capillary chromatography（MECC）. Homogeneity and stability monitoring of Baohuoside Ⅰpurity 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 BaohuosideⅠpurity CRM was 99.7%with expanded uncertainty of 0.3%（k=2）.
出处
《化学分析计量》
CAS
2014年第2期1-5,共5页
Chemical Analysis And Meterage
基金
国家科技支撑计划(21–09–4GZ–13)
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
Baohuoside Ⅰ purity CRM
development
high performance liquid chromatography
micellar electrokinetic capillary chromatography
uncertainty evaluation
