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目的:通过UPLC-ESI-Orbitrap-MS技术对绞股蓝总皂苷提取物的主要化学成分进行分析。方法:采用Thermo Q Exactive四极杆-静电场轨道阱高分辨质谱-色谱联用系统分析,以Hypersil Gold C_(18)色谱柱(2.1 mm×150 mm,1.9μm)为固定相,流动相0.1%甲酸水溶液(A)-乙腈(B)梯度洗脱(0~2 min,5%B;2~15 min,5%~95%B;15~17 min,95%B),流速0.3 mL·min~(-1),柱温40℃;质谱条件采用电喷雾离子化(ESI)方式,在负离子模式下,以Full Scan/Targeted-dd MS2扫描模式检测,研究绞股蓝总皂苷提取物的主要皂苷类化学成分。结果:通过与对照品比对、结合参考文献,分析多级质谱数据,根据化学成分的质谱碎片,推测色谱峰对应的化学结构,共归属8种具有原人参二醇型母核结构的绞股蓝皂苷,分别是绞股蓝皂苷Ⅲ,Ⅳ,Ⅷ,Ⅻ,Rg_3,Rb_2,Rc,Rf。结论:该研究采用的方法简单、快速、灵敏,对绞股蓝总皂苷提取物中具有原人参二醇型母核结构的主要皂苷类进行了高分辨质谱分析,这一方法可以从定性分析的角度,对市售绞股蓝总皂苷提取物的质量进行初步快速鉴别。
OBJECTIVE: To analyze the main chemical constituents of gypenosides extract by UPLC-ESI-Orbitrap-MS. Methods: A Hypersil Gold C_ (18) column (2.1 mm × 150 mm, 1.9 μm) was used as the stationary phase and the mobile phase 0.1 was analyzed by Thermo Q Exactive Quadrupole Electrostatic Field Orbitrap High Resolution Mass Spectrometry- (0-2 min, 5% B; 2-15 min, 5% -95% B; 15-17 min, 95% B) with a flow rate of 0.3 mL · mL min -1, and the column temperature was 40 ℃. The mass spectrometry conditions were determined by ESI-ESI-MS. In the negative ion mode, the total saponin of gypenosides extract was detected by Scanning-Targeted-dd MS2. Chemical composition. Results: The chemical structure of the corresponding chromatographic peaks was deduced by comparing with the reference substance and the reference data, analyzing the mass spectrometry data, and inferring the chemical structure corresponding to the chromatographic peak according to the chemical composition. Eight kinds of gypenosides , Respectively, gypenosides Ⅲ, Ⅳ, Ⅷ, Ⅻ, Rg_3, Rb_2, Rc, Rf. Conclusion: The method used in this study is simple, rapid and sensitive. The main saponins with protopanaxadiol nuclei structure in Gypenosides extract were analyzed by high resolution mass spectrometry. This method can be used qualitatively and qualitatively. The quality of the commercially available gypenosides extract initial rapid identification.