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不同石斛枫斗中酚酸类活性成分的比较及杓唇石斛素和石斛酚含量的测定

周婧1,2, 许志良2,3, 孔宏伟2*, 路鑫2, 许国旺2   

  1. 1. 沈阳药科大学药学院, 辽宁 沈阳 110016; 2. 中国科学院大连化学物理研究所分离分析重点实验室, 辽宁 大连 116023; 3. 浙江中医药大学, 浙江 杭州 310053
  • 收稿日期:2010-01-25 修回日期:2010-03-25 出版日期:2010-06-28 发布日期:1980-06-25
  • 通讯作者: 孔宏伟

Comparison of phenolic components among different species of Dendrobium (Shihu Fengdou) and determination of their active components—moscatilin and gigantol

ZHOU Jing1,2, XU Zhiliang2,3, KONG Hongwei2*, LU Xin2, XU Guowang2   

  1. 1. School of Pharmacy, Shenyang Pharmaceutical University, Shenyang 110016, China; 2. Key Laboratory of Separation Science for Analytical Chemistry, Dalian Institute of Chemical Physics, Chinese Academy of Sciences, Dalian 116023, China; 3. Zhejiang Chinese Medical University, Hangzhou 310053, China
  • Received:2010-01-25 Revised:2010-03-25 Online:2010-06-28 Published:1980-06-25
  • Contact: KONG Hongwei

摘要: 建立了基于液相色谱-离子阱飞行时间串联质谱(LC-IT-TOF MS/MS)的酚酸类分析方法,对6种共18批次的石斛枫斗药材中的酚类化合物进行了研究,其中18种酚酸类化合物得到初步定性。在共有化合物中选择杓唇石斛素和石斛酚作为质量控制的目标化合物。在此基础上,采用响应面法(RSM)确定了提取溶剂为60%甲醇、提取时间为65 min的超声提取杓唇石斛素和石斛酚的最佳条件,建立了石斛枫斗中杓唇石斛素、石斛酚的高效液相色谱(HPLC)含量测定方法。定量线性优于0.999 8,检出限(LOD)分别为0.18 mg/L和0.09 mg/L,重复性的相对标准偏差(RSD)小于3%,加标回收率均值分别为97.1%和101.4%。这些结果表明本研究建立的方法可用于石斛枫斗药材中酚酸类化学成分研究及质量控制。

关键词: 杓唇石斛素, 酚酸类物质, 含量, 石斛酚, 石斛枫斗 , 液相色谱-离子阱飞行时间串联质谱

Abstract: A liquid chromatography coupled with ion trap-time of flight mass spectrometry (LC-IT-TOF MS/MS) profiling method was developed for the analysis of the phenolic constituents in Dendrobium. Six different species of Dendrobium were analyzed. Eighteen phenolic constituents in the samples were tentatively identified based on their mass spectra and related literatures. Moscatilin and gigantol were chosen as potential quality control targets of all species of Dendrobium. A high performance liquid chromatography (HPLC) method was developed for quantitative analysis of moscatilin and gigantol in Dendrobium. The extraction condition for moscatilin and gigantol was optimized by the response surface methodology (RSM). The linearity of the method is more than 0.9998 and the precision is within 3% for all the two analytes. The limits of detection (LOD) were 0.18 mg/L and 0.09 mg/L respectively. Recoveries were 97.1% and 101.4% respectively. The study might provide a basis for the quality control of Dendrobium.

Key words: content, Dendrobium (Shihu Fengdou) , gigantol, moscatilin, phenolic components, liquid chromatography-ion trap-time of flight mass spectrometry (LC-IT-TOF/MS)