摘要
全二维气相色谱(GCxGC)是九十年代发展起来的分离复杂混合物的一种全新手段。自1991年其思想及其装置问世后,得到了迅速的发展。
本论文首先以石油产品为样品研究了全二维气相色谱-飞行时间质谱(GCxGC-TOFMS)的特性,讨论了柱系统的匹配、调制条件等对分离的影响,并提出了柱系统优化的策略及两维分辨率的概念,
为GCxGC用于解决复杂样品分析提供了技术基础。
在上述研究的基础上,本论文首次应用GCxGC-TOFMS于中药挥发油的研究。首先优化了适合中药挥发油分析的柱系统和操作条件,并考察了用于指纹分析的适用性和方法学。以三种挥发油为例,
基于多次调制(定性)信息,加上两维保留时间和峰纯度数据,鉴定了其中的重要组分,含量累加均超过90%。进一步对广藿香进行研究,药效成分得以完全分离和正确定量。评价中药挥发油的3种方法得以建立,
其中根据族分离特性的用药效分子群代替个别药效组分评价中药质量的方法充分体现了中药的复杂性和中医用药的整体性。最后以姜黄挥发油的快速族组成分析为例,显示GCxGC在中药挥发油筛选和质控中的应用前景。
GCxGC is a novel separation method for complex samples emerging in the 1990's. After the idea was prompted and implemented, it is experiencing rapid development.
In the thesis, we firstly demonstrated characteristics of GCxGC-TOFMS using petroleum samples, discussed influence of column match and modulation conditions on separation, and gave a strategy of system optimization and suggested the concept of two dimensional resolution, providing technological foundation for separation of complex samples.
On the above basis, GCxGC-TOFMS was applied to study volatile oils of Traditional Chinese Medicines (TCMs). Column system and operation conditions were optimized. Applicability of GCxGC and its methodology for TCMs was investigated. Components of three volatile oils were identified with 2D Rts, peak purity and multiple modulation information from TOFMS, concentration sums of which were more than 90% for each sample. Further study of patchouli was carried out with curative components completely separated and accurately quantified. Three assessing methods of TCMs were suggested; especially the method based on effective group separation can reflect the complexity and the entirety of TCMs to the most. With GCxGC alone, fast group identification of a curcuma volatile oil was achieved, which indicates the prospective of GCxGC to screening and quality control of TCMs.
引文
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