胡椒碱分离纯化工艺的研究
Separation and purification process of piperine
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摘要: 以胡椒碱粗提物为研究对象,通过静态和动态实验,对适合分离纯化胡椒碱的大孔树脂进行筛选,确定大孔树脂分离胡椒碱的最佳工艺条件。将分离纯化的胡椒碱浓缩液进行重结晶,得到胡椒碱单体,确定最佳重结晶条件。结果表明:HPD-800大孔树脂分离纯化胡椒碱效果最好,动态实验最佳工艺参数为上样液浓度1.6mg/m L,p H自然,上样量30m L,上样流速80m L/h,洗脱液甲醇体积分数50%,p H3,体积50m L,在此条件下得到胡椒碱旋干物的纯度为82%。最佳重结晶条件为:胡椒碱浓度200mg/m L、自然p H、0℃下重结晶24h。该条件下得到的胡椒碱单体纯度≥96%,再次结晶后其纯度可达99%。Abstract: Based on static and dynamic adsorption performance, HPD-800 type macroporous resin was selected as a more appropriate carrier to separate and purify piperine from crude extract of piperine by ultrasonic.Then, recrystallize the concentrated piperine solution. The optimal process parameters for dynamic adsorption and desorption were determined as follows:30m L of 1.6mg/m L samples at natural p H and 80 m L/h of loading flow rate, followed by desorption with 50 m L 50% methanol at p H3.0. Under this condition, the purity of piperine was 82%. The purity of piperine could reach 96% at the optimal process parameters for recrystallization:piperine concentration was 200mg/m L, natural p H, 0℃ recrystallize for 24 h. Recrystallize again, the purity could up to 99%.