H103大孔吸附树脂分离纯化苦参碱与氧化苦参碱

通过对比苦参总碱在9种大孔树脂上的静态吸附,筛选出对苦参总碱吸附能力较强的H103树脂;研究了H103树脂对上述两种生物碱的吸附等温曲线及吸附动力学行为;考察了苦参总碱在H103树脂上的动态吸脱附过程,用薄层色谱法(TLC)对洗脱液跟踪分析,用高效液相色谱法(HPLC)检测苦参碱、氧化苦参碱含量,确定了动态吸脱附的过程参数。结果表明,H103树脂对苦参总碱的等温吸附可采用Freundlich方程描述;由吸附动力学曲线得H103树脂在100 min内达到平衡,具有较快吸附速度,吸附动力学规律可用二级速率方程表示;动态吸脱附过程的洗脱条件为:用体积分数30%乙醇-体积分数25%氨水(体积比115∶1),体积分数80%乙醇梯度洗脱,氧化苦参碱先被洗脱,苦参碱随后,两种生物碱可达到很好的分离,经计算苦参碱收率为90.1%,氧化苦参碱收率为85.3%。

Separation and Purification of Matrine and Oxymatrine with H103 Macroporous Resin

The static adsorption properties of alkaloids in nine kinds of macroporous resins were evaluated.The H103 macroporous resin which displayed the best adsorption capacity among the tested resins was picked out;the adsorption isotherm curve and adsorption kinetic behaviour of alkaloids with H103 macroporous resin were systematically studied,and the dynamic adsorption and desorption capability of alkaloids on H103 resin-packed column was investigated to establish optimal parameters for separation of matrine and oxymatrine.The different eluent was detected by thin layer chromatography(TLC),and the sample of matrine or oxymatrine was detected by high performance liquid chromatography(HPLC).The results show that the adsorption isotherm could be described by Freundlich isotherm equation.According to the dynamic adsorption curve,the balance time was 100 minutes;the adsorption kinetic law could be expressed by quasi-second-order-rate equation;the optimized dynamic process for gradient elution was 30% CH3CH2OH-25% NH3·H2O(115∶ 1,V/V) and 80% CH3CH2OH;the oxymatrine was eluted firstly with a recovery yield of 85.3%,then matrine was eluted with a recovery yield of 90.1%.These two alkaloids could be separated effectively.