人参、红参皂苷类成分指纹图谱研究

为了建立一种快速鉴定人参和红参的方法，应用超高效液相色谱-串联质谱研究人参和红参中的皂苷类成分指纹图谱。室温下用甲醇提取人参粉末，提取液离心，并用0.22 μm滤膜过滤。色谱柱是BEH Shield RP₁₈ 柱( 1.7 μm×2.1×50 mm, Waters ,USA)和BEH保护柱；流动相：乙腈（A），水（B）；0~5 min A从25%到50%，5~8 min，A从50%变化到90%，8~10 min，A从90%变到100%，10~12 min，A保持在100%；进样体积10 μL，检测波长195 nm。质谱喷雾电压-4.5 kV，金属毛细管电压-45 V，温度250 ℃，壳气（氮气）流速27 L/h，辅助气（He）流速180 L/h，质量扫描范围m/z 200~1 500，碰撞气为氦气，质谱碎裂信息用来鉴定皂苷。液质联用数据显示在人参炮制过程中化学成分发生了变化，结果表明不同批次的人参与红参能够清晰分组。该方法快速，简单，特征性和重现性良好。

Fingerprint Study on Ginsenoside in Ginseng and Red Ginseng

A rapid analysis method was established to identify ginseng and red ginseng. Ginsenosides in ginseng and red ginseng were studied as the fingerprint compounds by ultra-high performance liquid chromatography-electrospray ionization multistage tandem mass spectrometry (UPLC-ESI-MSⁿ). Power of ginseng sample was extracted with methanol at room temperature. The extract was centrifuged and filtered through a 0.22 μm filter before analyzed by UPLC-MS. UPLC separations were carried out using a BEH Shield RP₁₈ column (1.7 μm×2.1×50 mm, Waters ,USA) and a BEH RP₁₈ guard column(Waters). The column temperature was kept at 25 ℃. The flow rate was set to 0.3 mL/min， and the eluting gradient was as follows: acetonitrile (A) and water (B)]: 0—5 min, 25%—50%A; 5—8 min,50%—90% A; 8—10 min, 90%—100% A;10—12 min, 100%A. The injection volume was 10 μL. The detection wavelength was 195 nm. The mass spectrometer was operated in the negative ion mode with source voltage of 4.5 kV. The metal capillary voltage was 45 V, and temperature was 250 ℃. The sheath gas(N₂) flow-rate was 27 L/h, the auxiliary gas (He) flow-rate was 180 L/h. The scan range was m/z 200—1 500. Helium was used as collision gas, and collision energy was adjusted for the intensity ratio of the base peak to the parent ion between 2 and 20. The fragments got from ESI-MSⁿ supplied very important information to identify the ginsenosides. The data of the UPLC-ESI-MSⁿ for ginseng samples and red ginseng samples revealed that the chemical composition changes during the red ginseng steaming process. The result shows different batches of ginseng and red ginseng are clearly distinguished, which explain the chemical composition changes during the red ginseng steaming process. The method is rapid, simple, characteristic and good reproducibility.