杜仲中环烯醚萜类化合物的快速制备色谱制备及反相高效液相色谱/核磁共振鉴定

建立了杜仲中环烯醚萜类化合物京尼平甙酸(GPA)和京尼平甙(GPS)的快速制备色谱制备及反相高效液相色谱/核磁共振(RP-HPLC/NMR)鉴定方法。杜仲皮醇提物用硅胶柱层析法纯化后,进行快速制备液相色谱分离,根据制备色谱图收集流出液,采用HPLC-PDA和核磁共振(NMR)法定性定量分析。制备色谱条件为:流动相,V(甲醇)∶V(水)∶V(乙酸)=40∶60∶0.5;流速,2.5 mL/m in;检测波长,254 nm;进样体积,2.5 mL;进样量,100 mg;柱温,室温。结果表明,RP-HPLC分析制得产品的质量分数分别为w(GPA)=94.69%和w(GPS)=93.27%,核磁共振法测定结果与文献报道一致,确定实验所得两种单体为京尼平甙酸和京尼平甙。

Preparation and Identification of Iridoid Glycosides in Eucommia ulmoides Olive by Preparation Chromatography,Resversed Phase High Performance Liquid Chromatography and Nuclear Magnetic Resonance

The method using preparation chromatography,resversed-phase high performance liquid chromatography and nuclear magnetic resonance(RP-HPLC/NMR) for the preparation and identification of the iridoid glycosides——geniposidic acid(GPA) and geniposide(GPS) in Eucommia ulmoides Olive was established.After the plant was extracted with ethanol-water,the crude extract was purified by silica gel column.Then preparative liquid chromatography was used to isolate GPA and GPS according to the chromatogram.The samples were identified by HPLC-PDA and NMR.The preparation conditions were:column,Pure 2811C_(18),250 mm×8 mm;mobile phase,V(methanol)∶V(water)∶V(acetic acid)=40∶60∶0.5;detection wavelength,254 nm;flow rate,2.5 mL/min;volume of injecting sample,2.5 mL;quantity of injecting sample,100 mg;column temperature,room temperature.The results showed that purities of the products were w(GPA)=94.69% and w(GPS)=93.27%.NMR experiments indicated that the two monomers were identical to GPA and GPS.