反相制备液相色谱同时分离制备独一味中4种环烯醚萜苷类化合物

Simultaneous isolation and preparation of four iridoid glycosides from Lamiophlomis rotata by preparative RP-HPLC

目的建立独一味中环烯醚萜苷类化合物山栀苷甲酯、螃蟹甲苷II、番木鳖苷和8-O-乙酰山栀苷甲酯的快速制备色谱方法。方法独一味水提物经聚酰胺色谱柱和大孔吸附树脂柱分离后,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和质谱定性定量分析。结果质谱法确定实验所得4种单体分别为山栀苷甲酯、螃蟹甲苷II、番木鳖苷和8-O-乙酰山栀苷甲酯,RP-HPLC法分析质量分数分别为95.7%、94.8%、96.3%、98.2%。结论该分离方法中各组分分离效果较好,可用于独一味中4种环烯醚萜苷类化合物的分离制备。

Objective To establish a gradient preparative chromatography,RP-HPLC,and mass spectrometry（MS） method for the preparation and identification of four iridoid glycosides from Tibetan medicinal herb Lamiophlomis rotata.Methods After the plant was extracted with water,the crude extract was purified by polyamide column and macroporous adsorptive resins column.Then preparative liquid chromatography was used to isolate shanzhiside methylester,phloyoside II,loganin,and 8-O-acetyl-shanzhiside methylester.The samples were identified by HPLC and MS.Results MS determination indicated that the four monomers were identical to be shanzhiside methylester,phloyoside II,loganin,and 8-O-acetyl-shanzhiside methylester.The results showed that purities of the products were 95.7%（shanzhiside methylester）,94.8%（phloyoside II）,96.3%（loganin）,and 98.2%（8-O-acetyl-shanzhiside methylester）,respectively.Conclusion The method has good separative effect.It is suitable to be used for the prepared separation of four iridoid glycosides from L.rotata.