摘要
目的 建立超高效液相色谱串联—四极杆—静电场轨道阱质谱技术(ultra-performance liquid chromatogra-phy-linear ion trap quadrupole-Orbitrap-mass spectrometry,UPLC-Q-Orbitrap-MS)对铁皮石斛(Dendrobiumoffi-cinale Kimura&Migo)水提物石油醚、乙酸乙酯、正丁醇3种萃取组分进行定性表征的方法.方法 提取铁皮石斛水提物并依次用石油醚、乙酸乙酯、正丁醇萃取,旋蒸浓缩后,得到石油醚、乙酸乙酯、正丁醇萃取组分.样品经UPLC-Q-Orbitrap-MS分析,根据元素组成、分子量、质荷比、离子碎片等确定化合物信息并推导裂解规律,通过与文献、MzCloud、MzVault、PudChem、本地数据库比对确定鉴定结果.结果 在正负离子模式下共鉴定出化合物62种,包括黄酮类成分20种,联苄类成分6种,羧酸及其衍生物6种,脂肪酸及其衍生物6种,酚类成分4种,氨基酸及其衍生物3种,糖类成分2种,生物碱类、苯丙素、蒽醌、萜类化合物各1种,其他类成分3种,还检测到8种含量较高、质谱信号较强的未知成分.其中水提石油醚萃取物中鉴定出化合物7种,乙酸乙酯萃取物中鉴定出化合物36种,正丁醇萃取物中鉴定出化合物48种.通过与文献比对,62种化合物中有7种化合物为首次从铁皮石斛中提取得到.结论 该方法可快速有效分析铁皮石斛中多种化学成分,可为铁皮石斛质量控制及药效物质基础研究提供参考.
Abstract
Objective To establish a method based on ultra-performance liquid chromatography-linear ion trap quadrupole-Orbi-trap-mass spectrometry (UPLC-Q-Orbitrap-MS)for qualitative characterization of the extraction components of petroleum e-ther,ethyl acetate,and n-butanol in water extracts of the traditional Chinese medicine Dendrobium officinale.Methods The water extracts of Dendrobium officinale were obtained and sequentially extracted with petroleum ether,ethyl acetate,and n-butanol,and the extraction components of petroleum ether,ethyl acetate,and n-butanol were obtained after concentration by rotary evaporation.The samples were analyzed and processed by UPLC-Q-Orbitrap-MS to determine the information of com-pounds based on elemental composition,molecular weight,mass-to-charge ratio,and fragment ions and to deduce the cleavage pattern,and the compounds were identified by comparison with the literature,MzCloud,MzVault,PudChem,and local data-bases.Results A total of 62 compounds were identified in positive and negative ionmodes,including 20 flavonoid components, 6 bibenzyl components,6 carboxylic acids and their derivatives,6 fatty acids and their derivatives,4 phenolic components,3 a-mino acids and their derivatives,2 glycan components,1 each of alkaloids,phenylpropanoids,anthraquinones,and terpenoids, and 3 other types of components,and 8 unknown components were also detected with a relatively higher level and strong mass spectrometry signals.Seven compounds were identified in the petroleum ether extract,36 compounds were identified in the eth-yl acetate extract,and 48 compounds were identified in the n-butanol extract.By comparison with the literature,among these 62 compounds,7 were reported for the first time from Dendrobium officinale.Conclusion This method can rapidly and ef-fectively analyze multiple chemical components in Dendrobium officinale,which can provide a reference for the quality control of Dendrobium officinale and the basic research on medicinal substances.
基金项目
安徽省中医药科技攻关专项项目(202303a07020005)
国家自然科学基金联合基金项目(U19A2009)
国家自然科学基金青年科学基金项目(82304881)
维普
万方数据