基于HPLC-ESI-MS^(n)和指纹图谱结合化学计量评价不同生长年限铁皮石斛黄酮类成分差异  

Evaluation of Flavonoid Composition Differences in Dendrobium officinale of Different Growth Years Based on HPLC-ESI-MS^(n) and Fingerprint Analysis

作　　者：李运容 黄国东[1] 李锦妍 吴樟桦 陈松 黄月纯[3] 魏刚[2] LI Yunrong;HUANG Guodong;LI Jinyan;WU Zhanghua;CHEN Song;HUANG Yuechun;WEI Gang(International Zhuang Medicine Hospital,Affiliated to Guangxi University of Chinese Medicine,Nanning 530201,China;School of Traditional Chinese Medicine,Guangzhou University of Chinese Medicine,Guangzhou 510006,China;First Affiliated Hospital,Guangzhou University of Chinese Medicine,Guangzhou 510405,China)

机构地区：[1]广西中医药大学附属国际壮医医院,广西南宁530201 [2]广州中医药大学中药学院,广东广州510006 [3]广州中医药大学第一附属医院,广东广州510405

出　　处：《食品工业科技》2024年第18期239-249,共11页Science and Technology of Food Industry

基　　金：广西中医药大学博士启动基金资助项目(2018BS073);全国名中医黄汉儒学术思想及临床经验传承推广中心(2022V004);国家中医药管理局高水平中医药重点学科建设项目-少数民族药学(壮药学)(zyyzdxk-2023165);黄汉儒全国名中医传承工作室建设项目;黄瑞松全国名老中医药专家传承工作室。

摘　　要：目的:分析广西铁皮兰种铁皮石斛中的黄酮类成分,并探究不同生长年限对黄酮类成分积累的影响。方法:用Kromasil 100-5 C_(18)色谱柱(250 mm×4.6 mm,5μm),以乙腈-甲醇(v:v=1:1)-0.01 mol/L乙酸铵溶液为流动相进行梯度洗脱,质谱使用ESI离子源,在负离子模式下采集数据;采用HPLC法建立25批广西铁皮石斛HPLC特征图谱,并运用主成分分析和聚类分析探讨不同生长年限对广西铁皮石斛黄酮类成分积累的影响。结果:通过HPLC-ESI-MS^(n)技术,从广西铁皮石斛中鉴定了19个黄酮类成分,涵盖了黄酮碳苷(9个)、黄酮醇氧苷(4个)、酰化黄酮碳苷(2个)、酰化黄酮醇氧苷(3个)及二氢黄酮(1个)。构建了广西铁皮石斛黄酮类成分特征图谱,并指认了9个共有峰;基于聚类与主成分分析,将25份样品按生长年限及杆色(绿杆1~3年、绿杆3~5年、红杆1~3年、红杆3~5年)划分为四类。此外,黄酮类特征峰峰面积随着生长年限的增长而增长;在1~3年生长年限时,‘红杆’与‘绿杆’间黄酮含量无显著差异;但3~5年,红杆样品中新西兰牡荆苷Ⅰ、Ⅲ、佛莱心苷及特定峰(峰8、峰9)含量显著高于绿杆。结论:本研究通过质谱分析结合化学模式识别,揭示了广西铁皮石斛黄酮类成分的共有特征,并强调了生长年限对黄酮类成分积累的关键作用。特别指出,生长至3~5年,‘红杆’样品中黄酮类成分含量显著高于‘绿杆’,此发现为铁皮石斛的药理活性探索、应用开发、种质资源评价及采收策略提供了坚实的理论基础。Objective:To conduct an analysis of the flavonoids in Dendrobium officinale Kimura et Migo from Guangxi and to investigate the effects of different growth years on the accumulation of flavonoids.Methods:A Kromasil 100-5 C_(18) column(250 mm×4.6 mm,5μm)was used for chromatographic separation with a gradient elution of acetonitrile-methanol(v:v=1:1)-0.01 mol/L ammonium acetate solution as the mobile phase.Mass spectrometry data was collected using ESI ion source in negative ion mode.HPLC was used to establish the characteristic chromatographic fingerprints of 25 batches of Dendrobium officinale from Guangxi,and principal component analysis and cluster analysis were employed to investigate the effects of different growth periods on the accumulation of flavonoid components.Results:A total of 19 flavonoids were identified from Dendrobium officinale from Guangxi through the HPLC-ESI-MS^(n) technique,encompassing 9 flavonoid glycosides,4 flavonol glycosides,2 acylated flavonoid glycosides,3 acylated flavonol glycosides,and 1 dihydroflavone.The characteristic maps of flavonoids in Dendrobium officinale from Guangxi were established,and 9 common peaks were identified.Based on clustering and principal component analysis,25 samples were categorized into four classes in accordance with growth years and rod color(green rod for 1~3 years,green rod for 3~5 years,red rod for 1~3 years,red rod for 3~5 years).Additionally,the peak area of the characteristic peak of flavonoids increased with the increase of growth years.There was no marked difference in flavonoid content between the'red'and'green'during the 1~3 years of growth.Nevertheless,the contents of moscatin I,moscatin III,chrysin,and specific peaks(peak 8,peak 9)in the red rod samples were significantly higher than those in the green rod samples during the 3~5 years.Conclusion:In this study,leveraging mass spectrometry analysis integrated with chemical pattern recognition,elucidated the common characteristics of flavonoid compounds in Dendrobium officinale sourced from Gua

关 键 词：广西铁皮兰种 黄酮类成分 化学模式识别 品种 生长年限 

分 类 号：TS207.3[轻工技术与工程—食品科学]