基于UPLC-ESI-Orbitrap-MS技术对金钗石斛生物碱的分析
发布时间:2018-06-10 17:12
本文选题:金钗石斛 + 倍半萜类生物碱 ; 参考:《中国实验方剂学杂志》2017年20期
【摘要】: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。
[Abstract]:Aim: to analyze the main chemical constituents of Dendrobium nobile alkaloids by UPLC-ESI-Orbitrap-MS. Methods: Thermo Q active quadrupole and electrostatic field orbital trap high resolution mass spectrometry were used as stationary phase with Hypersil Gold C18 column 2.1 mm 脳 150 mm ~ (1.9 渭 m) as stationary phase, and Hypersil Gold C _ (18) column (2.1 mm 脳 150 mm ~ (1.9 渭 m) was used as stationary phase. The mobile phase (0.1% formic acid aqueous solution) was gradient eluted by AI-acetonitrile B) with a gradient elution of 0 ~ 2 min ~ 5 min ~ (5) and B ~ (95) B ~ (15) ~ (17) min ~ (95) B ~ (-1), the flow rate was 0.3 mL / L, the column temperature was 40 鈩,
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