高效液相色谱法测定钩藤中钩藤碱和异钩藤碱的含量  

Determining the Contents of Uncinine and Isuncinine in Uncaria by High Performance Liquid Chromatography

作　　者：李浩明 张楠楠 LI Hao-Ming;ZHANG Nan-Nan(National Center for Quality Inspection and Testing of Chinese Medicinal Materials,Bozhou 236800,China;Bozhou Products Quality Supervision and Inspection Institute,Bozhou 236800,China)

机构地区：[1]国家中药材产品质量检验检测中心,安徽亳州236800 [2]亳州市产品质量监督检验所,安徽亳州236800

出　　处：《中国药物经济学》2024年第5期97-100,共4页China Journal of Pharmaceutical Economics

摘　　要：目的 探讨采用高效液相色谱法(HPLC)测定钩藤中钩藤碱和异钩藤碱含量的可行性。方法 采用Thermo C_(18)(250×4.6 mm,5μm)色谱柱,以甲醇-0.2%氨水(65∶35)为流动相,流速:1.0 ml/min,柱温:30℃,检测波长:245 nm,进样量:20μl。结果 钩藤碱、异钩藤碱在0.01~0.05 mg/ml范围内线性关系良好(r=0.999 9);重复性实验RSD依次为2.0%、0.83%;加样回收率依次为100.5%和101.5%;钩藤碱检出限与定量限依次为0.5μg/ml、1.5μg/ml,异钩藤碱检出限与定量限依次为0.2μg/ml、0.5μg/ml;对照品和供试品溶液均在24 h内稳定。随机测定10批次钩藤样品,钩藤碱、异钩藤碱含量差异较大。同一批钩藤药材中,带钩茎枝、叶中异钩藤碱含量较高,钩、无钩茎枝、主干中异钩藤碱含量依次降低;带钩茎枝、主干中钩藤碱含量较高,无钩茎枝、钩、叶中钩藤碱含量依次降低。结论 本方法简便、准确、重复性好,可用于钩藤中钩藤碱和异钩藤碱的含量测定。除传统的药用部位带钩茎枝外,钩藤其他部位均含有钩藤碱和异钩藤碱。Objective To investigate the feasibility of determining the contents of uncinine and isuncinine in uncaria by high performance liquid chromatography(HPLC).Methods The chromatography was performed on Thermo C_(18)(250×4.6 mm,5 μm)column with methanol-0.2% ammonia water(65∶35) as the mobile phase,the flow rate was 1.0 ml/min,the column temperature was 30 ℃,the detection wavelength was 245 nm,and the sample size was 20 μl.Results The linear relationship between leucine and isoleucine was good in the range of 0.01~0.05 mg/ml(r=0.999 9).RSD of repeatability experiments were 2.0% and 0.83%respectively.The recoveries were 100.5% and 101.5% respectively.The limits of detection and quantitation of unguine were 0.5 μg/ml and 1.5 μg/ml respectively,and the limits of detection and quantitation of isunguine were 0.2 μg/ml and 0.5 μg/ml respectively.Both the control product and the test product were stable within 24 h.The contents of crotonine and iso-crotonine in 10batches of crotonine samples were different.In the same batch of uncinaria,the content of isoparinine was higher in the stem branches and leaves with uncinaria,but decreased in the stem branches without uncinaria and trunk.The content of unhooked stems and stems was higher than that of unhooked stems,unhooked stems and leaves.Conclusion The method is simple,accurate and reproducible,and can be used for the determination of uncinine and isuncinine in uncaria.In addition to the traditional medicinal parts with uncinaria stems and branches,other parts of uncinaria contain uncinine and isuncinine.

关 键 词：钩藤 钩藤碱 异钩藤碱 含量测定 高效液相色谱法 方法学验证 

分 类 号：R284.1[医药卫生—中药学]