高效液相色谱-离子阱-飞行时间质谱鉴定决明子化学成分  

Components identification in Cassiae Semen by HPLC-IT-TOF MS

作　　者：骆宜 张乐[1] 王卫华[2] 刘斌[1] 

机构地区：[1]北京中医药大学,北京100102 [2]中国计量科学研究院,北京100013

出　　处：《药物分析杂志》2015年第8期1408-1416,共9页Chinese Journal of Pharmaceutical Analysis

基　　金：北京中医药大学自由选题项目(2015-JYB-XS107)

摘　　要：目的:建立高效、准确鉴定决明子中化学成分的液质联用方法。方法:采用高效液相色谱-离子阱-飞行时间质谱(HPLC-IT-TOF MS)联用技术,在电喷雾离子源的正、负离子模式下,以甲醇-乙腈(21)混合溶液(A)-水(B)梯度洗脱,流速为1.0 m L·min-1,柱温为35℃。根据决明子的一级和二级质谱图,对比对照品保留时间并结合文献,推测化合物可能的裂解途径和结构。结果:通过分析各组分质谱数据,共鉴别了17个化合物,包括7个萘并吡喃酮类化合物、7个蒽醌类化合物和3个萘酚类化合物,其中有决明子内酯龙胆二糖苷为首次从该植物中发现。结论:采用IT-TOF MS技术有利于新化合物的发现和鉴别,为中药化学成分、质量控制研究提供了新内容。Objective：To develop a facile method for identification of components in Cassiae Semen by HPLC-MS. Methods：The method was performed on HPLC-IT-TOF MS with electrospray ionization in both positive and negative ion modes with the mobile phase of mixed solution of methanol and aeetonitrile in proportion 2 ： 1 （A） -water （B） by gradient elution. The column temperature was at 35 ℃ and the flow rate was 1.0 mL . min - 1. According to first and multi-stage mass spectrum diagrams, retention time of standard materials and published reports, the components in Cassiae Semen were identified and their fragmentation pathways were concluded. Results： A total of 17 components were identified, including 7 naphthopyrones, 7 anthraquinones and 3 naphthols. Among them, cassia- lactone gentiobioside was found for the first time in Cassiae Semen. Conclusion ： The application of IT-TOF MS in determining components in TCM is useful and will provide essential data for further research.

关 键 词：离子阱-飞行时间质谱 决明子 化学成分 结构鉴定 药效物质基础 裂解途径 

分 类 号：R917[医药卫生—药物分析学]