Isolation And Structural Identification Of Chemical Constituents From Traditional Chinese Medicine

The medicinal plant Cortex dictamni is the drying root of Dictamn dasycarpus Turcz and Dictamnus angustifolius GDon. It is a common herbs and widely distributed in Asia. Modern pharmacological studies had showed that Cortex dictamni existing heat-clearing, damp-drying, antioxidant, antiviral, antibacterial, anti-inflammatory, anti-tumor, protect liver, and other pharmacological effects according to the related literatures, and more pharmacological effects of Cortex dictamni remain to be further research. In this paper the chemical constituents of Cortex dictamni from taibai mountain in Shannxi province were studied, and ten kinds of compounds were separated and identified from it, including a new compound named dictamformal. The root bark of Cortex dictamni was collected from taibai mountain and reduced big roots to powder, it was extracted by methanol soaking method, and the active ingredients were enriched. Afterwords, the extractions were dissolved by hydrochloric acid of 0.3% concentration, the acid dissolving part and acid insoluble part were obtained. Then acid dissolving was adjusted the pH to 9 with ammonia, extracted with methylene chloride getting the non-alkaloid methylene chloride layer. The acid insoluble part was suspended and washed with water, extracted with methylene chloride, ethyl acetate and n-butanol getting the acid insoluble part methylene chloride layer, ethyl acetate layer, N-butyl alcohol layer. The alkaloid methylene chloride layer and acid insoluble part methylene chloride layer were separated carefully by the thin-layer chromatography and column chromatography. Ten kinds of compounds were isolated from Cortex dictamni, the compounds were identified by the one-dimensional nuclear magnetic resonance 1H-NMR 13C-NMR, two-dimensional nuclear magnetic resonance 1H-1H COSY, HSQC, HMBC, NOESY and the HRESIMS techniques. Their structures were identified as fraxinellone, dictamine, Oxidation fraxinellone, obacunone, preskimmianine, hydroxylation fraxinellone, limonin, dictamformal, trigonelline and y-fagarine. Among them dictamformal was a new conpound that isolated from Cortex dictamni. This paper was divided into the following three parts:1. Introduction. The species and distribution of Cortex dictamni were introduced in this chapter. The chemical compositions that separated from the Cortex dictamni and the current pharmacological effects of extraction that proved by all kinds of experiments were also introduced in the chapter one.2. The extraction and separation of chemical constituents of Cortex dictamni. The process of collection, dry and extraction of Cortex dictamni were introduced in this chapter. The root bark of medicinal plant Cortex dictamni was reduced big root to powder, then it was extracted by methanol soaking method. Afterwords, the extractions were dissolved by 0.3% concentration of hydrochloric acid, the acid dissolving part and acid insoluble part were obtained. Then acid dissolving was adjusted the pH to 9 with ammonia, extracted with methylene chloride getting the non-alkaloid methylene chloride layer. The acid insoluble part was suspended and washed with water, extracted with methylene chloride, ethyl acetate and n-butanol getting the acid insoluble part methylene chloride layer, ethyl acetate layer, N-butyl alcohol layer. First of all, the conditions of column chromatography were selected using different solvents and different proportions of solvents, afterwards, The alkaloid methylene chloride layer and acid insoluble part methylene chloride layer were separated carefully by the thin-layer chromatography and column chromatography. Ten kinds of compounds were obtained from Cortex dictamni.3. The identification of the chemical constituents isolated from Cortex dictamni. Ten kinds of pure compounds were isolated from the Cortex dictamni, and then the structure of constituents were determined by by the one-dimensional nuclear magnetic resonance 1H-NMR,13C-NMR, two-dimensional nuclear magnetic resonance 1H-1H COSY, HSQC, HMBC, NOESY and the HRESIMS techniques, and ten compounds structure were obtained, including fraxinellone, dictamine, oxidation fraxinellone, obacunone, preskimmianine, hydroxylation fraxinellone, limonin, dictamformal, trigonelline and y-fagarine, Among them the dictamformal was a new conpound that isolated from Cortex dictamni. In the future the active point, pharmacological action and clinical effect of the ten compounds can be studied, and we can also establish a high performance liquid chromatography (HPLC) method for determining the content of active ingredients in Cortex dictamni.