| Z Schinifolium Sieb.et. Zucc. and Z Bungeanun Maxim. are major varieties of Z Schinifolium L.in china. Both of them contain large amount of numb taste components. Z Schinifolium Sieb.et. Zucc. has a taste of fragrance and numb taste components in it have staying power, while the taste of Z Bungeanum Maxim., is more mellow and heavier. However, during the storage, the numb taste components lose a lot. There exists mark decrease in fragrance and tingling feeling in crusted Z Schinifolium.Studying the trend of change in the content of numb taste components and change mechanism in Z Schinifolium can provide the basis for the quality control of Z Schinifolium and its products.Fresh Z Schinifolium Sieb.et. Zucc. and Z Bungeanum Maxim are adopted as raw materials in this paper. By HPLC, the effects of different meshes, temperatures and packing methods on qualities of Zanlhoxylum hungeanum Maxim and Zanthoxylum schinifolium Sieb. et Zucc. were studied. And then chromatography and other methods were adopted to isolate, purify the numb-tasted components of Zanthoxylum L., Then the extracts were dealt with different methods and the changed extract were isolated, purified and identified. During the process, the substance was prelimilarily determined and the mechanism of degration of numb taste components was realized, which at the same time provided the basis for related research. The main results are as follows:1. HPLC was used to study the trend of change in the content of numb taste components in Z Schinifolium Sieb.et. Zucc. and Z Bungeanum Maxim during6months. The effects of different meshes, temperatures and packing methods were shown in the trend. (1) The results showed that the content of numb taste components in Zanthoxylum bungeanum Maxim and Zanthoxylum schinifolium Sieb. et Zucc were differed, where existed significant difference(P<0.05). The content of dried pericaps of Zanthoxylum schinifolium Sieb. et Zucc was60.15mg/g. The other was only20.15mg/g.(2) The whole pericarps of Zanthoxylum L. were prone to store than powered pericarps. Temperatures and packing methods also lead to significant difference (P<0.05) in numb taste components of Zanthoxylum L..(3) Within a range, low storage temperatures were benefit to stabilities of Zanthoxylum L. Aluminum foil materials with vacuum package were the best packing method in storages of Zanthoxylum L., which could hold60per of the numb tastecomponents even stored in40℃.2. A series of extraction and separation and purification methods were adopted to get pure numb taste components in Zanthoxylum L., whose relative content reach97.7%.(1) Separation and purification process of the numb-tasted components of Zanthoxylum L.Powered pericarps of Zanthoxylum L.'Soxhlet extraction method'The counter-current dry column chromatography'Preparation of HPLC purification(2) Three peaks, all of which are white crystal suspensions after concentration, were got through pre-HPLC.GC-MS was adopted to detect the components in them. Results showed that the relative content of numb taste components in them separately are98.45%、66.94%and neally100%. A substance occupied97.7%in the3rd peak.(5) The3rd peak was deteced by LC-MS and NMR. It was hydroxyl-β-sanshool. The structure was as follows:3. When studying the changed numb taste components, hydroxyl-β-sanshool was dealed with different methods. Then the sensory properties of the changed components were observed. Chromatography and mass spectrography were used to purify and detect the changed components so that the changed structure and mechanism could be known. The results were as follows:(1) Hydroxyl-β-sanshool was exposed to air, low tempreture, UV and some other conditions. Results showed that it changed fastest under oxygen and UV condition and the effective components were detected little after exposed6h under UV conditions by HPLC.(2) By HPLC, the changed hydroxyl-β-sanshool was separated by gradient elution. Both of the peaks which covered largest area showed biggest absorbtion at224nm.(3) Through pre-HPLC, two major components of changed hydroxyl-β-sanshool were got. GC-MS detection found that the relative content of279reached62.22%and33.88%seperatly. In the2nd peak, there exits another substance whose molecular weight was261, covering an area of31.88%.(4) The two peaks were deteced by LC-MS. The relative molecular mass was279and261. According to the mass spectrogram showed in GC-MS, references and reaction conditions, the structure of the two substanced were proposed. The1st substance whose relative molecular mass was279may be the oxidation product of hydroxyl-β-sanshool, whose right side of the double bond of the conjugated double bonds structure was oxidated. The1st substance losed one H2O molecule on the right and then the2nd substance was got during the seperation. The structures were as follows:... |
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