摘要
目的:采用超高效液相色谱-四级杆-飞行时间串联质谱法(UPLC-Q-TOF-MS/MS)技术分析吴茱萸药材中的化学成分。方法:色谱条件为ACQUITY UPLC BEH C18色谱柱(2.1 mm×100 mm,1.7μm),流动相乙腈(A)-0.1%甲酸水溶液(B)梯度洗脱(0~3 min,6%A;3~4 min,6%~10%A;4~7 min,10%~12%A;7~8 min,12%~14%A;8~13 min,14%~15%A;13~15 min,15%~20%A;15~18 min,20%~30%A;18~21 min,30%~49%A;21~25 min,49%~51%A;25~27 min,51%~73%A;27~30 min,73%~80%A;30~31 min,80%~100%A;31~32 min,100%A),流速0.4 mL·min^(-1),柱温35℃。质谱条件为电喷雾离子源,正、负离子全扫描模式采集数据,检测范围m/z 100~1200。通过高分辨质谱数据分析、参考文献数据及对照品确认,对吴茱萸药材的化学成分进行快速、全面的定性分析。结果:从吴茱萸70%甲醇提取物中共鉴定出92个化合物,包括生物碱类39个、黄酮类19个、柠檬苦素类12个、酚酸类20个和有机酸类2个;通过与对照品比对,准确归属了26个化合物。结论:吴茱萸药材化学成分类型多样,极性差异大,但不同产地、不同品种的药材样品中化学成分基本一致。该研究建立的方法能快速、准确地对吴茱萸的化学成分进行全面解析,为该药材药效成分和毒性成分的进一步阐明提供了实验依据。
Objective:To analyze the chemical constituents in Euodiae Fructus by ultra-high performance liquid chromatography quadrupole time-of-flight mass spectrometry(UPLC-Q-TOF-MS/MS).Method:The chromatographic separation was performed on an ACQUITY UPLC BEH C18 column(2.1 mm×100 mm,1.7μm)with acetonitrile(A)-0.1% formic acid aqueous solution(B)as mobile phase(0-3 min,6%A;3-4 min,6%-10%A;4-7 min,10%-12%A;7-8 min,12%-14%A;8-13 min,14%-15%A;13-15 min,15%-20%A;15-18 min,20%-30%A;18-21 min,30%-49%A;21-25 min,49%-51%A;25-27 min,51%-73%A;27-30 min,73%-80%A;30-31 min,80%-100%A;31-32 min,100%A)for gradient elution.The column temperature was 35℃,and the flow rate was 0.4 mL·min^(-1).Mass spectrometry was performed using an electrospray ionization and data were collected in positive and negative ion modes,and the detection range was m/z 100-1200.The chemical constituents in Euodiae Fructus were identified rapidly and comprehensively based on the accurate relative molecular mass and combined with literature data and reference substances.Result:A total of 92 chemical constituents were speculatively identified from the 70% methanol extract of Euodiae Fructus,including 39 alkaloids,19 flavonoids,12 limonoids,20 phenolic acids and 2 organic acids.Among them,26 compounds were confirmed by the reference substances.Conclusion:The compound types of Euodiae Fructus are multiple and quite different in polarity.The chemical compositions of Euodiae Fructus from different regions and species are similar.The established method is rapid and accurate,with which the chemical compositions of Euodiae Fructus have been identified comprehensively.Therefore,this study provides an experimental reference for further clarifying active and toxic constituents of Euodiae Fructus.
作者
赵晓梅
程宇欣
梁彩霞
郭杰
刘晓谦
冯伟红
赵正保
闫利华
王智民
ZHAO Xiao-mei;CHENG Yu-xin;LIANG Cai-xia;GUO Jie;LIU Xiao-qian;FENG Wei-hong;ZHAO Zheng-bao;YAN Li-hua;WANG Zhi-min(Shanxi University of Chinese Medicine,Jinzhong 030619,China;National Engineering Laboratory for Quality Control Technology of Chinese Herbal Medicines,Institute of Chinese Materia Medica,China Academy of Chinese Medical Sciences,Beijing 100700,China;Shanxi Medical University,Taiyuan 030001,China)
出处
《中国实验方剂学杂志》
CAS
CSCD
北大核心
2021年第6期113-126,共14页
Chinese Journal of Experimental Traditional Medical Formulae
基金
国家“重大新药创制”科技重大项目(2018ZX09721-004-001)
国家公益性行业科研专项(201507002)
国家自然科学基金项目(31200244)
中央级公益性科研院所基本科研业务费专项(ZXKT17063)。
