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 chromatography-linear ion trap quadrupole-Orbitrap-mass spectrometry,UPLC-Q-Orbitrap-MS)对铁皮石斛(Dendrobium officinale 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。
Objective To establish a method based on ultra-performance liquid chromatography-linear ion trap quadrupole-Orbitrap-mass spectrometry(UPLC-Q-Orbitrap-MS)for qualitative characterization of the extraction components of petroleum ether,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 compounds 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 databases.Results A total of 62 compounds were identified in positive and negative ion modes,including 20 flavonoid components,6 bibenzyl components,6 carboxylic acids and their derivatives,6 fatty acids and their derivatives,4 phenolic components,3 amino 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 ethyl 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 effectively 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.
作者
李金淼
解会群
姚亮
韩岚
彭代银
LI Jinmiao;XIE Huiqun;YAO Liang;HAN Lan;PENG Daiyin(School of Pharmacy,Anhui University of Chinese Medicine,Anhui Hefei 230012,China;Institute of Traditional Chinese Medicine Resources Protection and Development,Anhui Hefei 230012,China;Synergetic Innovation Center of Anhui Authentic Chinese Medicine Quality Improvement,Anhui Hefei 230012,China;Anhui Key Laboratory of Modern Chinese Materia Medica,School of Pharmacy,Anhui University of Chinese Medicine,Anhui Hefei 230012,China)
出处
《安徽中医药大学学报》
CAS
2024年第4期92-99,共8页
Journal of Anhui University of Chinese Medicine
基金
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)。
关键词
铁皮石斛
超高效液相串联—四极杆—静电场轨道阱质谱技术
化学成分
定性分析
Dendrobium officinale
Ultra-performance liquid chromatography-linear ion trap quadrupole-Orbitrap-mass spectrometry
Chemical components
Qualitative analysis