| Modern medicine regimen is gradually developed, based on the traditional Chinese medicine theory of "treat-pre-disease", Chinese medicine has a great advantage in the treatment of sub-health and the prescription of four green granules is from the folk prescription. Polygonal, Longan, Wolfberry and so on in the prescription are all "medicine food homology" medicine, having the effect of anti-fatigue, enhance memory, and improve immune function and so on, which have been widely used in folk. This topic will improve formulation into granules using modern technology, and establish its quality control standards and conduct research on moisture resistance.Objective:1, To identify the original medicine and effective components of Four Tonic Green Granules, and control production process of four green tonic particle resulted by layer chromatography to provide the basis of qualitative identification of four tonic green particles.2, To establish the method of determining the content of diosgenin by HPLC chromatography.3, To prepare granules with strong moisture resistance using critical relative humidity method, and select the proper excipients.Method:1, Thin layer chromatography(TLC):Polygona and granules in the prescription are qualitatively identified with petroleum ether (60?90 ?)- ethyl acetate-formic acid (5:2:0.1) as developing solvent using silica gel GF254.2, HPLC chromatography:The content of diosgen in tonic green particles is determined by HPLC chromatography. The HPLC system consists of Waters-C18 column (4.6 mm × 250 mm,5 ?m), and mobile phase of pure acetonitrile, with the flow rate of 1mLˇmin-1, detection at 204nm, column temperature of 25 ?, injection volume of 20?l.3, Critical relative humidity(CRH):Microcrystalline cellulose, lactose, mannitol, soluble starch, maltose, sorbitol and ?-cyclodextrin is respectively mixed with extract with the ratio of 4:1, and the mixture is respectively blended, sieved, granulated; particles will be spread evenly on the tray and put into the oven with the temperature of 60 ? for half an hour; then granulate and dry them again. At the same time, draw moisture absorption curve of all kinds of excipient to analyze the data,with time as the abscissa, moisture absorption rate as the ordinate, in order to prepare granules with strong wet resistance, evaluated with the indexes of moisture content, forming rate and appearance.Results:1, Polygonal and granules are identified by TLC with clear spots and good resolution, and its results show remarkable effectiveness in identification (Rf=0.6).2. HPLC, the determination of content of the diosgenin, shows that the linear range is from 0.256?4.56 ?g/ˇmL-1, R2=0.9997, with an average recovery of 101.40%, RSD of 1.50%(n=9), and repeatability of 1.43%(n=9). The content of 3 batches of diosgenin is 0.29?0.32 ug/g.3. The order of the saturated moisture content of each excipient is listed as follows: lactose< mannitol< microcrystalline cellulose< beta cyclodextrins<soluble starch< sorbitol< maltose. The optimal formulation is the mixture of extract and hybrid materials (MCC:lactose=1:1.5) with the ratio of 1:4, screened by the properties, appearance and moisture content of granular.Conclusion:1. TLC is simple and has clear spots which can qualitatively and preliminarily identify all the medicinal substances in the prescription of Four Tonic Green Granules.2. HPLC, established for the determination of the content of diosgenin in the Four Tonic Green Granules, is simple, accurate, exclusive, and has good reproducibility. It also provides a basic measurement for diosgenin in the Four Tonic Green Granules, and can be considered as one of control means for the quality of the Four Tonic Green Granules.3. Critical relative humidity(GRH), established for the detemination of the wet resistance of excipient, is simple, and provides the basis for the preparation of Four Tonic Green Granules with strong wet resistance. |
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