摘要
目的建立离子交换树脂纯化.HPLC分析方法用于同时测定山豆根中苦参碱和氧化苦参碱含量。方法山豆根药材提取液经阳离子交换树脂柱纯化后,以C-18化学键合硅胶为固定相,流动相为乙腈-0.2%磷酸-三乙胺(8:92:0.01;V/V/V),检测波长208nm。结果在本文建立的分析条件下。苦参碱和氧化苦参碱的色谱保留时间分别约为5.5min和8.1min,10min内可完成1次分离分析过程。苦参碱进样浓度在1.0~300.0μg·ml-1范围与峰面积线性关系良好(r2=0.9996)。氧化苦参碱进样量在2.0~600.0μg·ml-1范围与峰面积线性良好(r2=0.9998)。苦参碱、氧化苦参碱平均测定回收率分别为90.5%和91.6%,方法已应用于同时测定不同产地山豆根药材中苦参碱和氧化苦参碱含量。结论山豆根样品经纯化分离后,苦参碱、氧化苦参碱与药材中其余内源性物质分离完全,定量准确.方法适用于山豆根药材质量控制及其药品含量检测。
Objective To purificate matrine and oxymatrine in Sophora tonkinensis Gagnep. by ion exchange res- in and to establish a method for determining the two components by RP-HPLC. Methods The separation was performed on a -18 column with a mobile phase composed of acetonitrile-0.2 % phosphoric acid solution-triethanolamine (8: 92:0.01; V/V/V ) after the sample was extracted and purified with ion exchange resin. The detection wavelength was set at 208 nm. Results Matrine and oxymatrine had a retention time of approximately 5.5 min and 8.1 min, respectively. The peak shape was clear and symmetrical, and the analysis time was about 10 min per injection. Good linear correlations were ob- served when the amount of injection ranged from 1.0 to 300.0 0μg ·ml-1 for matrine ( r 2 =0. 9996) and 2. 0 to 600.0 μg·m1-1 for oxymatrine( r 2 =0. 9998). The average recovery of matrine and oxymatrine was 90.5% and 91.6% respec- tively for the Sophora tonkinensis Gagnep. samples. Conclusion A simple HPLC method has been established and valida- ted for simultaneous analysis of matrine and oxymatrine in Sophora tonkirtensis Gagnep.
出处
《解放军药学学报》
CAS
2014年第1期55-57,共3页
Pharmaceutical Journal of Chinese People's Liberation Army
基金
军队医疗机构制剂标准提高科研专项重点课题
No.13ZJZ13