高效液相色谱-离子阱-行时间质谱鉴定决明子化学成分

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 mL·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 acetonitrile 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, cassialactone 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.