基于超高效液相色谱串联四极杆静电场轨道阱质谱法的天麻眩晕宁颗粒化学成分鉴定及归属  

Identification and Attribution of Chemical Components in Tianma Xuanyunning Granules Based on UPLC-Q-Exactive Orbitrap MS

作　　者：吴健 关永霞 范建伟 张贵民 WU Jian;GUAN Yongxia;FAN Jianwei;ZHANG Guimin(Guangdong Pharmaceutical University,Guangzhou 510000,China;State Key Laboratory of Integration and Innovation of Classic Formula and Modern Chinese Medicine,Lunan Pharmaceutical Group Co.,Ltd.,Linyi 276006,China)

机构地区：[1]广东药科大学,广东广州510000 [2]鲁南制药集团股份有限公司经方与现代中药融合创新全国重点实验室,山东临沂276006

出　　处：《中国现代中药》2025年第4期647-660,共14页Modern Chinese Medicine

基　　金：山东省重点研发计划(重大科技创新工程)项目(2021CXGC010508)。

摘　　要：目的:采用超高效液相色谱串联四极杆静电场轨道阱质谱法(UPLC-Q-Exactive Orbitrap MS)对天麻眩晕宁颗粒的化学物质基础进行系统解析和归属,并探讨其化学成分的裂解规律。方法:采用Waters ACQUITY UPLC HSS T3色谱柱(100 mm×2.1 mm,1.8μm),流动相为0.1%甲酸水溶液(A)-乙腈(B),梯度洗脱(0~20.0 min,5%~30%B;20.0~23.0 min,30%~40%B;23.0~26.0 min,40%~70%B;26.0~27.0 min,70%~90%B;27.0~30.0min,90%B;30.0~30.5min,90%~5%B;30.5~35.0min,5%B),流速为0.3m L·min^(-1),柱温为30℃,进样量为2μL,质谱正、负离子模式扫描。采用Xcalibur 4.2软件分析得到化合物的精确质荷比、二级质谱裂解碎片等信息,并结合对照品比对和文献数据进行化合物解析,分析其裂解规律。结果:从天麻眩晕宁颗粒中共鉴定得到180个化合物,包括黄酮类53个、萜类35个、含氮类29个、有机酸类25个、酚类18个、苯酞类7个、其他类13个,并完成上述180个成分的全部归属,白芍、甘草、天麻归属到的成分较多,依次为50、49和26个。结论:所建立的方法能快速、准确地鉴定天麻眩晕宁颗粒中的化学成分,可为天麻眩晕宁颗粒物质基础研究提供依据,为质量控制提供参考。Objective:The ultra-high performance liquid chromatography tandem quadrupole electrostatic field orbital trap mass spectrometry(UPLC-Q-Exactive Orbitrap MS)technology was used to systematically analyze and classify the chemical basis of Tianma Xuanyunning Granules and explore the fragmentation patterns of its chemical components.Methods:Waters ACQUITY UPLC HSS T3 chromatography column(100 mm×2.1 mm,1.8μm)was used;the mobile phase was 0.1%formic acid aqueous solution(A)-acetonitrile solution(B)for elution gradient(0-20.0 min,5%-30%B;20.0-23.0 min,30%-40%B;23.0-26.0 min,40%-70%B;26.0-27.0 min,70%-90%B;27.0-30.0 min,90%B;30.0-30.5 min,90%-5%B;30.5-35.0 min,5%B).The volume flow rate was 0.3 mL·min^(-1),and the column temperature was 30℃.The injection volume was 2µL,and mass spectrometry scanning was performed in positive and negative ion modes.By using Xcalibur 4.2 software,precise mass-to-charge ratio,secondary mass spectrometry fragmentation,and other information were obtained and combined with a comparison of reference materials and literature data for compound analysis,so as to analyze its fragmentation patterns.Results:A total of 180 compounds were identified,including 53 flavonoids,35 terpenoids,29 nitrogen-containing compounds,25 organic acids,18 phenols,7 phthalides,and 13 other components.All 180 compounds were classified,with the top three medicinal herbs being Radix Paeoniae Alba,Radix et Rhizoma Glycyrrhizae,and Rhizoma Gastrodiae.The corresponding compounds were 50,49,and 26,respectively.Conclusion:The established method can quickly and accurately identify the chemical components in Tianma Xuanyunning Granules,providing a basis for the basic research of Tianma Xuanyunning Granules and a reference for quality control.

关 键 词：天麻眩晕宁颗粒 超高效液相色谱串联四极杆静电场轨道阱质谱法 化学成分 成分归属 

分 类 号：R284[医药卫生—中药学]