An ultrasonic extraction technology of preparing catalpol from Radix Rehmanniae was optimized by a uniform experimental design.The optimum conditions for ultrasonic extraction were thus established: 68% (vol) ethanol ...An ultrasonic extraction technology of preparing catalpol from Radix Rehmanniae was optimized by a uniform experimental design.The optimum conditions for ultrasonic extraction were thus established: 68% (vol) ethanol aqueous solution as extraction solvent,the volume(ml) to mass(g) ratio of extraction solvent to feed of 5∶1,the ultrasonic treatment time of 36 min.The crude catalpol obtained from the optimized ultrasonic extraction technology was further purified by selective adsorption with macroporous resin.The adsorption capacities and desorption yields of ten kinds of macroporous resins for catalpol were investigated.The results showed that H103 resin possessed the best performance.The properties of dynamic adsorption and desorption of H103 resin for catalpol were subsequently investigated on adsorption column.The optimum conditions for adsorption and desorption were determined.The concentration of catalpol in the loaded sample solution was 6.15 mg·ml-1,the flow rate was 1.0 ml·min-1,the volumetric percentage of ethanol in the eluting solvent was 75%,the elution flow rate was 0.5 ml·min-1 and the elution volume was 3.33 BV(bed volume).Under the above conditions,the purity of catalpol product eluted from the column packed with H103 resin reached 62.39% while that of the crude catalpol was only 10.01%.展开更多
以甲酸和氢氧化钾为原料,不外加任何溶剂一步合成二甲酸钾。通过单因素实验,考察了原料配比、反应温度和反应时间对产品质量与收率的影响。采用正交实验进一步优化了合成工艺,确定了最佳工艺条件:n(HCOOH)/n(KOH)=2.2、反应温度70℃、...以甲酸和氢氧化钾为原料,不外加任何溶剂一步合成二甲酸钾。通过单因素实验,考察了原料配比、反应温度和反应时间对产品质量与收率的影响。采用正交实验进一步优化了合成工艺,确定了最佳工艺条件:n(HCOOH)/n(KOH)=2.2、反应温度70℃、反应时间30 m in,在该条件下,二甲酸钾产品收率达98%以上。所得产品经红外光谱分析及熔点测定,其结果与文献报道一致。反应过程绿色化,有很好的原子经济性。展开更多
文摘An ultrasonic extraction technology of preparing catalpol from Radix Rehmanniae was optimized by a uniform experimental design.The optimum conditions for ultrasonic extraction were thus established: 68% (vol) ethanol aqueous solution as extraction solvent,the volume(ml) to mass(g) ratio of extraction solvent to feed of 5∶1,the ultrasonic treatment time of 36 min.The crude catalpol obtained from the optimized ultrasonic extraction technology was further purified by selective adsorption with macroporous resin.The adsorption capacities and desorption yields of ten kinds of macroporous resins for catalpol were investigated.The results showed that H103 resin possessed the best performance.The properties of dynamic adsorption and desorption of H103 resin for catalpol were subsequently investigated on adsorption column.The optimum conditions for adsorption and desorption were determined.The concentration of catalpol in the loaded sample solution was 6.15 mg·ml-1,the flow rate was 1.0 ml·min-1,the volumetric percentage of ethanol in the eluting solvent was 75%,the elution flow rate was 0.5 ml·min-1 and the elution volume was 3.33 BV(bed volume).Under the above conditions,the purity of catalpol product eluted from the column packed with H103 resin reached 62.39% while that of the crude catalpol was only 10.01%.
文摘以甲酸和氢氧化钾为原料,不外加任何溶剂一步合成二甲酸钾。通过单因素实验,考察了原料配比、反应温度和反应时间对产品质量与收率的影响。采用正交实验进一步优化了合成工艺,确定了最佳工艺条件:n(HCOOH)/n(KOH)=2.2、反应温度70℃、反应时间30 m in,在该条件下,二甲酸钾产品收率达98%以上。所得产品经红外光谱分析及熔点测定,其结果与文献报道一致。反应过程绿色化,有很好的原子经济性。
