UHPLC-Q Exactive高分辨质谱联用法分析淫羊藿中的化学成分  

Chemical constituents research of Epimedii Folium by UHPLC-Q Extractive Hybrid Quadrupole Orbitrap MS

作　　者：曾浏希 黎雄[2] 王东[1] 李杨[2] 杨洪艳[2] 高路 ZENG Liuxi;LI Xiong;WANG Dong;LI Yang;YANG Hongyan;GAO Lu(School of Traditional Chinese Materia Medica,Shenyang Pharmaceutical University,Shenyang 110016,China;The Second Clinical Hospital,Guangzhou University of Chinese Medicine,Guangzhou 510120,China)

机构地区：[1]沈阳药科大学中药学院,辽宁沈阳110016 [2]广州中医药大学第二临床医学院,广东广州510120

出　　处：《沈阳药科大学学报》2023年第5期581-592,662,共13页Journal of Shenyang Pharmaceutical University

基　　金：广州中医药大学“双一流”与高水平大学学科协同创新团队(2021xk39);国家自然科学基金资助项目(82004407)。

摘　　要：目的采用UHPLC-Q Exactive四极杆-静电场轨道阱高分辨质谱联用技术鉴定分析淫羊藿药材成分。方法采用Thermo Hypersil GLOD C_(18)(100 mm×2.1 mm,1.9μm)色谱柱,体积分数0.1%甲酸水溶液-乙腈溶液为流动相进行梯度洗脱,流速为0.3 mL·min^(-1),柱温为40℃,电喷雾正、负离子模式扫描。结果共分析和鉴定出79个化合物,包括黄酮类、生物碱类、有机酸类和木脂素类化合物,其中16个化合物经与对照品比对鉴定。鉴定的黄酮类包括46个异戊烯基黄酮醇类化合物,异戊烯基黄酮醇类负离子模式二级特征碎片为m/z 367、351、513、353和323。初步鉴定化合物41、54、76、65和69为新的异戊烯基黄酮。结论淫羊藿中异戊烯基黄酮醇类多具有淫羊藿素或8-异戊烯基山奈酚苷元母核结构,该结果为淫羊藿成分的系统分析提供了数据支持。Objective To isolate and identify the chemical constituents from Epimedii Folium by using UHPLC-Q Extractive Hybrid Quadrupole MS spectrometry.Methods Epimedii Folium was isolated on a Thermo Hypersil GLOD C_(18)(100 mm×2.1 mm, 1.9 μm).The mobile phase was acetonitrile and water containing 0.1%formic acid by gradient elution.The constituents of Epimedii Folium were isolated and identified by HRMS in the positive and negative ion mode using both full scan and two stage threshold-triggered mass modes with ESI.Results Total of 79 compounds from Epimedii Folium were identified, including flavonoids, alkaloids, organic acid and lignans.Among them, 46 prenylflavonols compounds were identified.The characteristic ions of negative mode of prenylflavonols included m/z 367,351,513,353 and 323.The identified new prenylflavonols compounds of Epimedii Folium included compounds 41,54,76,65,69 and so on.Conclusion Most of the prenylflavonols have the structure of icaritin or desmethylanhydroicaritin aglycone mother nucleus, which provides technical support for the component analysis of Epimedium.

关 键 词：UHPLC-Q Exactive 淫羊藿 淫羊藿素 8-异戊烯基山奈酚 异戊烯基的黄酮醇类 

分 类 号：R917[医药卫生—药物分析学] R28[医药卫生—药学]