目的以制备反相高效液相-蒸发光散射检测(RP-HPLC-ELSD)法为基础,大量分离制备达玛烷-3β,12β,20,25-四醇(25-OH-PPD)差向异构体,比较间隔连续进样法和离线制备法大量分离制备25-OH-PPD差向异构体的制备效率,探寻出最佳的分离制备色谱...目的以制备反相高效液相-蒸发光散射检测(RP-HPLC-ELSD)法为基础,大量分离制备达玛烷-3β,12β,20,25-四醇(25-OH-PPD)差向异构体,比较间隔连续进样法和离线制备法大量分离制备25-OH-PPD差向异构体的制备效率,探寻出最佳的分离制备色谱法。方法分别对间隔连续进样法以及离线制备法在不同比例的流动相和不同进样量下对25-OH-PPD差向异构体分离制备情况进行了考察,通过比较制备效率、转移率等筛选出最佳的制备方法。结果 2种方法最佳分离制备色谱条件和制备结果:间隔连续进样法流动相为甲醇-水(83∶17),体积流量20 m L/min,进样质量浓度20 mg/m L,进样量1 m L,20(S)-25-OH-PPD的制备效率为18.01 mg/h,20(R)-25-OH-PPD的制备效率为35.36 mg/h;离线制备法流动相为甲醇-水(81∶19),体积流量20 m L/min,进样质量浓度200 mg/m L,进样量2.5 m L;20(S)-25-OH-PPD的制备效率为50.55mg/h,20(R)-25-OH-PPD的制备效率为51.93 mg/h。结论离线制备法分离制备效率优于小质量浓度间隔连续进样法,离线制备法操作简单,重现性好,制备量大,为25-OH-PPD差向异构体混合物的大量分离制备奠定了良好的基础。展开更多
Gypenosides, a series of dammarane-type saponins from Gynostemma pentaphyllum Makino, were hydrolyzed under 5％ H_2SO_4 catalysis to afford the title compound as a new secondary sapogenin in addition to panaxadiol and...Gypenosides, a series of dammarane-type saponins from Gynostemma pentaphyllum Makino, were hydrolyzed under 5％ H_2SO_4 catalysis to afford the title compound as a new secondary sapogenin in addition to panaxadiol and 2a-hydroxypanaxadiol. The crystals of the title compound were obtained from methanol solution and a colourless crystal with dimensions of 0.2 × 0.2 × 0.2 mm was used. C_(30)H_(50)展开更多
文摘目的以制备反相高效液相-蒸发光散射检测(RP-HPLC-ELSD)法为基础,大量分离制备达玛烷-3β,12β,20,25-四醇(25-OH-PPD)差向异构体,比较间隔连续进样法和离线制备法大量分离制备25-OH-PPD差向异构体的制备效率,探寻出最佳的分离制备色谱法。方法分别对间隔连续进样法以及离线制备法在不同比例的流动相和不同进样量下对25-OH-PPD差向异构体分离制备情况进行了考察,通过比较制备效率、转移率等筛选出最佳的制备方法。结果 2种方法最佳分离制备色谱条件和制备结果:间隔连续进样法流动相为甲醇-水(83∶17),体积流量20 m L/min,进样质量浓度20 mg/m L,进样量1 m L,20(S)-25-OH-PPD的制备效率为18.01 mg/h,20(R)-25-OH-PPD的制备效率为35.36 mg/h;离线制备法流动相为甲醇-水(81∶19),体积流量20 m L/min,进样质量浓度200 mg/m L,进样量2.5 m L;20(S)-25-OH-PPD的制备效率为50.55mg/h,20(R)-25-OH-PPD的制备效率为51.93 mg/h。结论离线制备法分离制备效率优于小质量浓度间隔连续进样法,离线制备法操作简单,重现性好,制备量大,为25-OH-PPD差向异构体混合物的大量分离制备奠定了良好的基础。
文摘Gypenosides, a series of dammarane-type saponins from Gynostemma pentaphyllum Makino, were hydrolyzed under 5％ H_2SO_4 catalysis to afford the title compound as a new secondary sapogenin in addition to panaxadiol and 2a-hydroxypanaxadiol. The crystals of the title compound were obtained from methanol solution and a colourless crystal with dimensions of 0.2 × 0.2 × 0.2 mm was used. C_(30)H_(50)
