摘要
[目的]采用超高效液相色谱-飞行时间质谱联用技术(UPLC-Q-TOF-MS/MS),初步确定26个道地产区及其他产地的共计78批次防风样本的质量差异标志物。[方法]采用电喷雾离子源进行正离子采集,使用Waters Acquity UPLC BEH C18柱,流动相以0.1%甲酸水、0.1%甲酸-乙腈进行梯度洗脱;通过质谱解析软件(Markerview)对数据进行主成分分析(PCA分析),依据同位素峰度比和精确质量数确定其分子式,对比二级图谱与对照品图谱,进行结构鉴定。结合防风体内物质基础以及生物活性报道,确定候选质量差异标志物,进一步分析候选质量差异标志物在防风道地产区和非道地产区的含量变化规律,确定质量差异标志物。[结果]鉴定或推断了不同产地防风中含量差异较大的10种主要活性成分,其中Ledeouriellol、亥茅酚、补骨脂素、花椒毒素可初步作为防风道地药材的质量差异标志物。[结论]该方法能够准确、快速找出一批化合物可以作为质量差异标志物,提供了新的道地药材质量评价指标研究策略。
[Objective]To identify Quality marker in 78 batches of Radix Saposhnikoviae from different origins by ultra performance liquid chromatography coupled with time-of-fight mass spectrometry(UPLC-Q-TOF-MS/MS).[Methods]The UPLC-Q-TOF-MS/MS and electrospray ion(ESI)source were applied for the analysis under the positive ion mode and separation was performed onWaters Acquity UPLC BEH C18 column(2.1 mm×100 mm,1.7μm),with a mobile phase using water with 0.1%formic acid(A)and acetonitrile with 0.1%formic acid(B)for gradient elution,potential Q-markers were filtered through PCA analysis of Markerview 1.2.1 software,in vivo substance basis research and bioactivity reports from literature.Then the formula of potential Q-markers were determined by accurate mass and isotopic abundance ratio.The structure identification is through the comparison of the reference and the secondary spectrum of the database.Finally,the Q-markers were determined preliminarily by analyzing changes of content between geo-authentic origins and other origins.[Results]Ten differential compounds were identified or inferred between different origins.The geo-authentic origin Q-markers were Ledeouriellol,hamaudol,psoralen and xanthotoxin.[Conclusion]UPLC-Q-TOF-MS/MS method which develops a new strategy can be used for selection of quality evaluation index.It is helpful to make quality evaluation of authentic medicinal materials.
作者
霍金海
刘亚娟
任晓蕾
孙国东
刘政
孙建峰
王伟明
HUO Jinhai;LIU Yajuan;REN Xiaolei;SUN Guodong;LIU Zheng;SUN Jianfeng;WANG Weiming(Institute of Chinese Materia Medica,Heilongjiang Academy of Chinese Medicine Sciences,Harbin 150036,China)
出处
《天津中医药大学学报》
CAS
2021年第1期112-118,共7页
Journal of Tianjin University of Traditional Chinese Medicine
基金
黑龙江省自然科学基金项目(LH2019H092)
国家中药材产业技术体系专项项目(CARS-21)。