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机构地区:[1]黑龙江省中医药科学院中药研究所,黑龙江哈尔滨150036
出 处:《中药材》2017年第5期1123-1129,共7页Journal of Chinese Medicinal Materials
基 金:国家自然科学基金(81503348);国家"重大新药创制"科技重大专项(2010ZX09102-138);哈尔滨市青年科技创新人才基金项目(2012RFOYSO42)
摘 要:目的:采用超高效液相色谱-四极杆飞行时间质谱(UPLC-Q-TOF/MS)联用技术对胡桃楸叶进行分析,鉴定其主要化学成分。方法:采用Waters Acquity UPLC BEH C_(18)色谱柱(100 mm×2.1 mm,1.7μm),以0.1%甲酸(A)-0.1%甲酸乙腈(B)为流动相梯度洗脱;质谱采用电喷雾(ESI)离子源,在正、负离子模式下采集数据,通过Peakview 2.0/Masterview 1.0及Markerview 1.2.1软件进行目标及非目标筛查化合物,依据精确质量数和同位素峰度比确定化合物分子式,通过对照品及数据库的二级谱图比对、裂解规律分析,结合已有文献报道,鉴定化合物结构式。结果:从胡桃楸叶中鉴定了35个化学成分,包括10个萘醌类化合物,4个二芳基庚烷类化合物,10个黄酮类化合物及11个其他类化合物。结论:该方法快速、准确,为胡桃楸叶的化学成分鉴定提供一种新的方法。Objective: To identify the major chemical constituents of leaves of Juglans mandshurica by ultra performance liquid chromatography coupled with time-of-flight mass spectrometry(UPLC-Q-TOF/MS).Methods: The separation was performed on Waters Acquity UPLC BEH C_(18) column(100 mm × 2.1 mm,1.7 μm),with a mobile phase using 0.1% formic acid(A)-acetonitrile with0.1% formic acid(B) for gradient elution; Q-TOF/MS and electrospray ion(ESI) source were applied for the analysis under the positive and negative ion modes.Target search and non-target search were performed by Peakview 2.0/Masterview 1.0 or Markerview 1.2.1 software.Then the formula of compounds were determined by accurate mass and isotopic abundance ratio from target screening function of software.Their structure were determined by analysis of MS/MS fragment or comparison with standard substances and references.Results: 35 major chemical compounds including ten naphthalene quinones,four diarylheptanoids,ten flavonoids and eleven other compounds were identified in leaves of Juglans mandshurica.Conclusion: UPLC-Q-TOF/MS method develops a new strategy which can identify the main chemical constituents from leaves of Juglans mandshurica rapidly and accurately.
关 键 词:液相色谱-四极杆飞行时间质谱 胡桃楸叶 化学组分 萘醌 黄酮
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