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目的:通过UPLC-ESI-Orbitrap-MS技术对金钗石斛生物碱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 C18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 m L·min~(-1),柱温40℃,进样量2μL;质谱条件采用电喷雾离子化(ESI)方式,在正离子模式下,以full scan/targeted-dd MS2扫描模式检测,研究金钗石斛生物碱的主要化学成分。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种倍半萜类金钗石斛生物碱,分别是石斛碱(dendrobine),mubironine B,石斛氨碱(dendramine),石斛醚碱(dendroxine),石斛酮碱(nobilonine),6-羟基金石斛碱(6-hydroxynobiline),N-异戊烯基石斛碱(N-isopentenyldendrobinium),N-异戊烯基-6-羟基石斛碱(N-isopentenyl-6-hydroxydendroxinium)。结论:建立了金钗石斛倍半萜类生物碱的主要化学成分的分析方法,为金钗石斛药材的鉴别及质量控制提供了科学依据。
OBJECTIVE: To analyze the main chemical components of the alkaloids from Dendrobium nobile by UPLC-ESI-Orbitrap-MS. METHODS: A Hypersil Gold C18 column (2.1 mm × 150 mm, 1.9 μm) was used as the stationary phase and the mobile phase consisted of 0.1% formic acid in water with 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 gradient elution from acetonitrile to acetonitrile at a flow rate of 0.3 m L · min ~ (-1), the column temperature was 40 ℃, and the injection volume was 2μL. The mass spectrometry conditions were detected by full scan / targeted-dd MS2 scan mode in positive ion mode by electrospray ionization (ESI) The main chemical composition of alkali. Results: By comparing with reference materials, analyzing the data of multi-level mass spectrometry, the chemical structure corresponding to the chromatographic peaks was speculated according to the mass fraction of chemical constituents. Eight kinds of sesquiterpenoid nobile dendrobium alkaloids were assigned, which were Dendrobine, mubironine B, dendramine, dendroxine, nobilonine, 6-hydroxynobiline, N-isopentenylglucamine N-isopentenyl dendrobinium, N-isopentenyl-6-hydroxydendroxinium. Conclusion: The main chemical constituents of the sesquiterpenoids of Dendrobium nobile Lindl. Were established, which provided scientific basis for identification and quality control of Dendrobium nobile Lindl.