HILIC-ESI-TOF/MS测定海龙中的多种成分及其特征指纹图谱研究

Identification of active components in Syngnathus acus by HILIC-ESI-TOF/MS and study on their specific fingerprint chromatograms

目的建立亲水色谱-电喷雾飞行时间质谱(HILIC-ESI-TOF/MS)联用技术用于海洋中药海龙多种化学成分快速鉴定及其特征指纹图谱的研究方法。方法以海龙水提物为研究对象,采用加速溶剂萃取法(ASE)对海龙样品进行提取制备,采用HILIC法对海龙水提物进行快速分离,ESI-TOF/MS法对海龙水提物中多种化合物进行鉴别,在对已知活性成分进行定量测定的基础上,建立海龙的HILIC特征指纹图谱。结果应用HILIC-ESI-TOF/MS鉴定出海龙水提物中的10种成分,对其中7种核苷类成分进行了定量测定;在对多批次海龙药材分析的基础上,建立了其HILIC特征指纹图谱,结合相似度分析实现了海龙的质量评价及其与不同海洋药物的正确区分。结论本研究为海龙真伪鉴别研究提供了一种新方法。

Objective To develop a new method based on hydrophilic interaction ehromatography-electrospray ionization-time of flight-mass spectrometry （HILIC-DAD-ESI-TOF/MS） for the rapid identification of the active components in Syngnathus acus and the development of their specific fingerprint chromatograms. Methods Samples were extracted by accelerated solvent extraction, and the extraction conditions were optimized. The developed HILIC-DAD-ESI-TOF/MS method was used to identify the components in water extract from S. acus, and a chromatographic fingerprint based on HILIC analysis was established. Results Ten compounds in S. acus extract could be primarily identified by HILIC-DAD-ESI-TOF/MS on-line detection, in which seven nueleosides were determined. The HPLC characteristic fingerprint was established on the basis of analysis on the multi batches of S. acus, which could be used to evaluate the quality ofS. acus combined with similarity calculation. Conclusion This method is simple and rapid, and is a powerful tool for the identification ofS. acus.