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作 者:周婧[1,2] 许志良[2,3] 孔宏伟[2] 路鑫[2] 许国旺[2]
机构地区:[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
出 处:《色谱》2010年第6期566-571,共6页Chinese Journal of Chromatography
基 金:国际科技合作项目(No.2007DFA31060);国家科技支撑计划(No.2006BAI11B07)
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65min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0.18mg/L和0.09mg/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。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 0.999 8 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.
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