| According to its cooperative theory and plenty of clinical practice experiences, traditional Chinese medicine (TCM) has made an unique and unsubstituted contribution to disease treating in the history of our nation and the world. In the modern society, TCMs are not only used for disease treatment, but also studied as a kind of valuable culture inheritance in order to give patients a better therapy. TCM could be classified as traditional Chinese herbal medicine and traditional Chinese patent medicine (TCPM). TCPM has complex chemical constituents and pharmacodynamic effects, while some of them might have side effects. The knowledges about the effective constituents and their pharmacological mechanisms in TCPM are limited due to short of exploiture in technologies and methods. This problem should be considered seriously and solved effectively nowadays. Xiaoyao Pill has been compiled in the Pharmacopoeia of People's Republic of China in 2005 edition, which is a kind of TCPM and made from Bupleurum scorzonerifolium Willd., Angelica sinensis (Oliv.) Diels., Paeonia lactiflora Pall., Atractylodes macrocephala Koidz., Poria cocos (Schw.) Wolf., Glycyrrhiza uralensis Fisch. and Mentha haplocalyx Briq.. It provides clinical treatment for symptoms including nonsmooth by liver and spleen depression, chest pain, dizziness and menstruation disorders. Xiaoyao Pill was selected to study in this thesis. The extraction, identified and quantitative analysis of the volatile components in Xiaoyao Pill were investigated. Besides, in order to provide useful information for the quality control of Xiaoyao Pill, gas chromatography fingerprints of Xiaoyao Pill come from different manufactories were established.There are two parts in the paper: the introduction which is the first chapter of the thesis and the experiment and results part from chapter 2 to chapter 4 is the second part.In the first chapter of this thesis, the research on traditional Chinese patent medicines, Xiaoyao Pill (including characteristic, chemical constituent and pharmacological effect of each Chinese herbal medicine), essential oil (including general character, composition, application, extraction method and analytical measure), fingerprint of traditional Chinese medicines (including definition, characteristic, research significance, research measure and application) are summarized in general.Extracting and analyzing the volatile components in Xiaoyao Pill were investigated in chapter 2 and chapter 3. In chapter 2, the volatile components from Xiaoyao Pill were extracted by hydrodistillation and analyzed by gas chromatography-mass spectrometry (GC-MS). Single factor experiment and orthogonal experiment were applied to optimize the extraction process. The best extraction efficiency was obtained by using a ratio of drug to water of 1:15, soaking time of 10 h at room temperature and distillation time of 11 h. Under the optimal conditions, the components of Xiaoyao Pill were separated on a Rxi-5ms capillary column and identified by MS. The result indicated that 53 components including aromatic compounds, terpenic compounds, terpene alcohol compounds, zingiberone compounds and aldehyde compounds were identified, and there was a classified discussion on these volatile components. The proposed method could be applied for analysis of volatile components from other traditional Chinese patent medicines, and it could also provide useful information for the basic study on gas chromatography fingerprint of Xiaoyao Pill and the quality evaluation of Xiaoyao Pill. In chapter 3, the ultrasonic nebulization extraction (UNE) was developed and applied to the extraction of volatile components from Xiaoyao Pill. Several parameters of ultrasonic nebulization extraction, including the sample particle size, solvent volume and extraction time, were studied and selected. As a result, 2.4 g sample with particle size of 80 mesh was extracted by 15 mL of n-hexane for 20 min with ultrasonic power of 35 W. The volatile components were analyzed by gas chromatography-mass spectrometry (GC-MS) under the optimal conditions and 57 compounds were identified. The precision, repeatability and stability of the proposed method were also studied. Compared with ultrasonic-assisted extraction (UAE) and hydrodistillation (HD) extraction, the proposed method was more efficient, faster and easier to be operated at room temperature with smaller sample and energy consumption. It is suggested that the ultrasonic nebulization extraction can be used as a novel alternative method for extracting volatile components from traditional Chinese patent medicine.Chromatographic fingerprint analysis is considered one of the most effective approaches for quality control in traditional Chinese medicines. The gas chromatography fingerprints of the volatile components in Xiaoyao Pill were established and studied in chapter 4. In this chapter, the volatile components from Xiaoyao Pill were detected by gas chromatography-flame ionization detector (GC-FID) after hydrodistillation extraction. The method demonstrated good precision, reproducibility and stability with the relative standard deviations (RSDs) of the retention times less than 0.31% and the relative peak areas less than 4.8%. The GC fingerprints of Xiaoyao Pill were established by analyzing 10 samples from different manufacturers and hierarchical cluster analysis was carried out. According to relative retention times, 23 common peaks were indicated. Furthermore, the discrimination of the samples from different manufacturers was achieved by hierarchical cluster analysis via recognizing the 10×23 data matrix. The GC fingerprints with hierarchical cluster analysis provide more comprehensive information for the quality control of Xiaoyao Pill. |
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