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作 者:秦伟瀚[1] 刘翔[1] 阳勇[1] 张小梅[1] 郭延垒[1] 刘飞[1] QIN Wei-han LIU Xiang YANG Yong ZHANG Xiao-mei GUO Yan-lei LIU Fei(Chongqing Academy of Chinese Materia Medica, Chongqing 400065, Chin)
机构地区:[1]重庆市中药研究院,重庆400065
出 处:《分析测试学报》2017年第3期312-318,共7页Journal of Instrumental Analysis
基 金:国家自然科学基金资助项目(30901964;81072997);国家重大新药创制重大新药专项项目(2013ZX0101108)
摘 要:应用超高效液相色谱-四极杆串联飞行时间质谱法(UPLC-Q-TOF-MS)对凉山虫草提取物的主要化学成分进行定性分析。采用Agilent SB-C_(18)(50 mm×4.6 mm,1.8μm)色谱柱,以0.1%甲酸水-乙腈溶液为流动相,梯度洗脱,流速0.25 m L/min,柱温30℃;质谱分析采用信息关联模式(IDA)正、负离子分别采集。应用Peak View软件的Formula Finder等功能、各色谱峰的质谱数据与数据库匹配结合各色谱峰的二级碎片裂解规律,共鉴定出27个化合物,其中8个为虫草中未曾报道物质;主要化学成分包括生物碱、糖苷、核苷、氨基酸等成分。该方法精确、可靠、高效,适用于凉山虫草成分的快速鉴定,为凉山虫草的开发利用以及阐明其药效物质基础提供了参考。A UPLC-Q-TOF-MS method was developed for the analysis and identification of main chemical constituents in the extract of Cordyceps liangshanensis, by an Agilent SB-C18(50mm×4.6mm,1.8μm) column with gradient elution using of 0.1% formic acid in water and acetonitrile as mobile phase at a flow rate of 0.25mL/min.The column temperature was set at 30℃.MS analysis was based on information associated mode(IDA) with positive and negative ions collection. By using feature of PeakView such as Formula Finder,matching the mass spectrometry data of each chromatographic peak in the database and the cleavage law of each peak′s level two fragment,total of 27 compounds in Cordyceps liangshanensis were identified,in which 8 compounds in Cordyceps substance had never been reported before. The main chemical constituents include alkaloids,glycosides,nucleosides,amino acids,etc. The method is accurate,reliable and efficient,and is suitable for the rapid identification of ingredients in Cordyceps liangshanensis. It provides a reference for the development and utilization of Cordyceps liangshanensis and clarification of its efficacy and material basis.
关 键 词:凉山虫草 UPLC-Q-TOF-MS 裂解规律 化学成分
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