节点文献
野菊米挥发性成分的提取及分析研究
Extraction and Analysis on Volatile Constituents from Bud of Flos Chrysanthemi Indici
【作者】 陈小梅;
【导师】 王丽丽;
【作者基本信息】 浙江工业大学 , 应用化学, 2006, 硕士
【摘要】 野菊米为野菊含苞未放的花蕾,经杀青烘干制成,具有清热解毒、清火明目等功效。野菊的主要有效成分为挥发油和黄酮类化合物。目前,对野菊花挥发油的研究已有一定的报道,但对野菊米挥发油的研究还未见报道。植物在不同生长时期其化学成分的种类与含量会不同,所以野菊米与野菊花的化学成分也会有较大差异。为进一步研究其药用价值,我们收集了不同产地的野菊米,提取其挥发油进行气相色谱/质谱(GC/MS)分析。并研究了顶空固相微萃取-气相色谱/质谱(HS-SPME-GC/MS)联用技术,闪蒸-气相色谱法(FD-GC)等技术来分析野菊米的挥发性成分。论文共分为五章。第一章,文献综述部分。通过文献查阅,对挥发油分析技术和野菊米、野菊花的国内外研究概况作了系统的综述。对样品的提取技术如水蒸汽蒸馏(SD)、超临界流体萃取(SFE)、固相微萃取(SPME)等,及分析检测技术如气相色谱、质谱等在挥发油分析中的应用作了总结。第二章,采用SD法提取-GC/MS对浙江遂昌、安徽黄山、云南产野菊米挥发油进行了定性定量分析。用GC/MS对用SD法萃取得到的野菊米挥发油化学成分进行了研究,确定了最佳GC分离条件,并进行了定性与定量分析。鉴定出各产地野菊米挥发油化学成分52-65种,分别占挥发油92-96%。并将云南产野菊米和野菊花挥发性成分作了对比,发现野菊米挥发油的倍半萜类成分明显高于野菊花挥发油。另外还探讨了超临界CO2流体萃取浙江遂昌产野菊米挥发油,并与SD法进行了对比。第三章,研究了应用HS-SPME-GC/MS技术分析安徽黄山产野菊米挥发性成分。确定了最佳萃取条件,并与SD法和超临界CO2流体萃取法提取-GC/MS的结果进行了对比。HS-SPME-GC/MS法分析鉴定出野菊米样品中主要成分35种,且每种成分变异系数小于11%,表明该技术适合挥发油和香精产品的挥发性和半挥发性化学成分分析。第四章,研究了应用FD-GC法分析安徽黄山产野菊米。确定了最佳闪蒸条件,共分离出132个峰,经保留时间定性,鉴定出24个主要成分。同时用该法对遂昌和云南产野菊米进行了分析。与前面三种技术相比,FD-GC分析野菊米挥发性成分更简便、样品用量更少、快速、高效,可适用于大量野菊米样品的质量评价。第五章,对论文的主要研究成果进行了总结并提出了论文的不足与值得再深入研究的问题。
【Abstract】 Bud of Flos Chrysanthemi Indici is a common traditional Chinese medicine(TCM), which is used as heat-clearing and detoxication, protection against the cold et al. The main effective constituents for Bud of Flos Chrysanthemi Indici are volatile oil and flavonoids. Though there are many reports on Flos Chrysanthemi Indici, there is not any report on Bud of Flos Chrysanthemi Indici. However, there may be significant differences between the contents of volatile constituents for both samples because of their different growing stage. In this dissertation, in order to study their medical values with their chemical components, volatile oil from Bud of Flos Chrysanthemi Indici collected from different origins were extracted by steam distillation (SD) and supercritical carbon dioxide fluid extraction. Then, their chemical components were identified and quantified by gas chromatography/mass spectrometry (GC/MS). Furthermore, the volatile constituents from Bud of Flos Chrysanthemi Indici were also analyzed by headspace solid-phase microextraction-GC/MS (HS-SPME-GC/MS) and flash distillation-GC (FD-GC).In the first chapter, current methods of extraction and analysis for volatile oil from Flos Chrysanthemi Indici and its Bud were briefly described. Then, the specific features of extraction techniques such as steam distillation (SD), supercritical fluid extraction (SFE), solid phase microextraction (SPME) and analysis techniques such as GC and GC/MS used in this field were discussed.In chapter 2, the volatile oils for Bud of Flos Chrysanthemi Indici from Suichang in Zhejiang, Huangshan in Anhui and Yunnan were extracted by SD. Then, the chemical constituents were separated and identified by GC/MS. The optimum GC separation condition was examed, and the components were quantitatively determined with normalization method. 92-96% components of volatile oil included 52-65 kinds of compounds were identified on the obtained chromatograms. Furthermore, comparative analysis on the volatile oil for Flos Chrysanthemi Indici and its Bud in Yunnan was carried out. The result suggested there were significant differences between the contents of chemical constituents for both volatile oil samples. Moreover the constituents of volatile oil from Bud of Flos Chrysanthemi Indici in Suichang obtained by SFC were also analyzed by GC/MS, and compared with those obtained by SD.In chapter 3, volatile oil for Bud of Flos Chrysanthemi Indici from Huangshan was extracted and analyzed by HS-SPME-GC/MS. The optimum extraction condition was examed, and thus obtained result was also compared with SD and SFC followed with GC/MS analysis. 35 compounds of volatile oil from Huangshan were identified, the R. S. D. were below 11%. This result suggests that SPME is quite suitable for analysis of the volatile and semi-volatile compounds in volatile oil.In chapter 4, volatile oil for Bud of Flos Chrysanthemi Indici from Huangshan was analyzed by flash distillation-GC. The optimum condition was examed at first. Then, 132 peaks were separated and 24 main peaks among them were identified by retention time. And Bud of Flos Chrysanthemi Indici from Suichang and Yunnan were also analyzed by FD-GC. The obtained result shows that compared with the previous three methods, FD-GC is a relatively simple, rapid, sensitive and solvent-free method for the analysis of the volatile compounds, especially suitable for the application to quality evaluation of the TCM.In the last chapter, the main results obtained from this research were summarized. Then, the problems to be considered for this research and the possible future trends in this field were also discussed.
【Key words】 Bud of Flos Chrysanthemi Indici; volatile oil; extraction; GC/MS; HS-SPME-GC/MS; FD-GC;