高级检索+

基于UHPLC–QTOF–MS技术的五倍子单宁成分分析

Analysis of Tannin of Galla chinensis by UHPLC– QTOF–MS

  • 摘要:
    目的 基于超高效液相色谱–四极杆飞行时间–质谱(UHPLC–QTOF–MS)技术分析五倍子中单宁成分,建立一种有效的五倍子单宁成分测定方法,并解析单宁的裂解规律。
    方法 使用高温和超声波辅助方法提取五倍子中的酚类化合物,基于二级质谱推定化合物的裂解途径。
    结果 共鉴定到20种化合物,包含14种没食子单宁、3种酚酸、2种没食子酸酯和1种黄烷醇。以高温121℃为提取条件,均未鉴定到分子质量高于1 500 Da的没食子单宁,而在超声波辅助提取的五倍子水提取液中,成功地检测到1–O–没食子酰基葡萄糖至14–O–没食子酰基葡萄糖,其中,超声功率1 500 W,提取温度65℃条件下,鉴定到更多的没食子单宁异构体。MS/MS图谱显示,五倍子单宁主要通过没食子酸、没食子酰基、糖苷、水、羧基的损失进行裂解。
    结论 本研究证明,超声波辅助提取条件下,应用UHPLC–QTOF–MS技术能够全面高效地分析五倍子中的单宁成分,本研究为富含单宁的植物的化学成分研究提供参考依据。

     

    Abstract:
    Objective To develop an effective method for characterizing tannin of Chinese gallnut by ultra-performance liquid chromatography–quadrupole time of flight mass spectrometry (UHPLC–QTOF–MS), and analyze the fragmentation behavior of gallotannins.
    MethodsHigh temperature and ultrasonic–assisted methods were implemented for extracting phenolic compounds from Chinese gallnut, and the fragmentation pathway of gollotannins were characterized by MS/MS spectrometry.
    ResultsA total of 20 compounds were identified, including 14 gallotannins, 2 gallagyl esters, 3 phenolic acids, and 1 flavanol. Gallotannins with molecular mass higher than 1500 Da were not identified when high temperature 121 ℃ was used as extract method, while they were successfully detected by the ultrasound extract method, including 1–O–galloyl–βD–glucose to 14–O–galloyl–βD–glucose. Under the conditions of ultrasonic power of 1 500 W and extraction temperature of 65 ℃, more gallotannin isomers were identified. The MS/MS spectrum showed that gallotannins were mainly decomposed by the loss of glucoside, gallic acid, galloyl, H2O and carboxyl.
    Conclusion In the study, UHPLC–QTOF–MS technology coupled with ultrasonic extraction methods have been proved to determine gallnut tannin comprehensively and efficiently. The identification of gallnut tannin and the analysis of their fragmentation mechanism can provide a reference for research on the chemical composition of other plants rich in tannin.

     

/

返回文章
返回