HPLC结合PDA、MS分离制备独一味中9种环烯醚萜苷

Isolation and Identification of Nine Iridoid Glycosides from Lamiophlomis rotata by HPLC Combining PDA and MS

目的:建立系统分离制备独一味中9种环烯醚萜苷类化合物单体的色谱方法,并结合PDA与质谱法对目标化合物进行定性鉴定。方法:采用甲醇-水梯度洗脱方式进行系统分离分析,根据色谱图收集流出液,流出液氮气吹干得到目标化合物,采用RP-HPLC测定相应化合物的质量分数,PDA、MS定性鉴定。结果:经RP-HPLC分析,部分目标化合物质量分数高于90%,PDA、MS最终确定9种环烯醚萜苷类化合物分别为:Phlorigidoside C(1)、Schismoside(2)、Sesamoside(3)、Shanzhiside methylester(4)、6-O-Acetyl shanzhiside methylester(5)、PhloyosideⅡ(6)、Penstemoside(7)、Loganin(8)、8-O-Acetyl shanzhiside methylester(9)。结论:该方法对各组分分离分析效果好,简单易行,可用于独一味中9种环烯醚萜苷类化合物的定性分析和制备。

Objective：To establish a rapid chromatographic method to separate the iridoid glycosides from Lamioplomis rotata,and to identify the target compounds with PDA and MS. Methods ： Methanol-water gradient elution was used to separate and analyze the target compounds. The fluid fractions were gathered according to the chromatogram and dried with the nitrogen airflow. The mass fractions of the target compounds were determined with RP-HPLC and the structures were identified with PDA and MS. Results ：The purity of some compounds exceeded 90% and these 9 compounds were identified as iridoid glycosides, which were Phlorigidoside C （ 1 ） , Sehismoside （ 2 ） , Sesamoside （ 3 ） , Shanzhiside methylester （4） , 6 -O-Acetyl shanzhiside methylester （ 5 ） , Phloyoside Ⅱ（ 6 ） , Penstemoside （ 7 ） , Loganin（8） and 8-O-Acetyl shanzhiside methylester（9）. Conclusion： The method is simple and practicable with high efficiency. It can be used to qualitative and quantitative analysis of the 9 iridoid glycosides in Lamiphlomis rotata and its preparations.