液相色谱-电喷雾离子阱质谱法快速鉴定刺五加提取物中的四种组分

Rapid Identification of Acanthopanax senticosus Mixture by Liquid Chromatography-Electrospray Ion Trap Mass Spectrometry

  • 摘要: 探讨了采用液相色谱 -电喷雾串联质谱法 ( L C-MSn,n=1~ 3 )检测刺五加中异秦皮定以及微量双环木脂素松脂醇 -二 -O-β-D-葡萄糖苷、刺五加苷 D和松脂醇的方法。流动相为甲醇 -水 ( 5 0∶ 5 0 ,体积比 )的混合液。色谱柱为 Diamonsil C18(内径 2 0 0 mm× 4.6mm,粒径 5μm) ,流速为 0 .5 m L/min。结果表明 :异秦皮定、松脂醇 -二 -O-β-D-葡萄糖苷、刺五加苷 D和松脂醇的准分子离子 ( M+H+ )和它们的 MS2 主碎片离子分别为 m/z 2 2 3、m/z 70 0、m/z 2 0 8、m/z 2 3 5、m/z 41 9和 m/z 2 3 5。该法可以应用于刺五加中异秦皮定和相关双环木脂素成分的鉴定

     

    Abstract: The method of reversed-phase high performance liquid chromatography-electrospray ionization tandem mass spectrometry (LC-ESI/MS n, n=1-3) for the rapid identification of isofraxidin and trace lignans, pinoresinol-di-O-β-D-glucoside, eleutherosides D and pinoresinol, in Acanthopananx senticosus Harms was established. The mixtures were successfully isolated on a Diamonsil C 18 column (200mm×4.6mm×5μm), using methanol-water (50∶50, v/v) as the mobile phase at a flow rate of 0.5mL/min. Compared with the LC-ESI-MS n spectra of standard samples, isofraxidin and three lignans in Acanthopanax senticosus mixture were identified. The results showed the quasimolecular ion and MS 2 main fragment ion peaks of isofraxidin, pinoresinol-di-O-β-D-glucoside, eleutherosides D and pinoresinol are m/z223(M(222)+H +), m/z700(M(682)+NH 4 +), m/z760(M(742)+NH 4 +) and m/z359(M(358)+H +), and m/z208, m/z235, m/z419 and m/z235, respectively.

     

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