| ObjectsThe project mainly studied the extracting, refining, concentration, drying and molding process of total saponins in ilicis asprellae, and to discuss the antiviral effection of total saponins on the basis of improving the quality standard of ilex asprella. The methods and results are as follows in detail:Methods1 Due to the present qulity standard of ilex asprella is weak, the subject established a TLC identification method and built a content determination method to improve the quality standard of ilicis asprellae.2 The preparation technology of total saponins from ilicis asprellae. firstly, With the retention rate of total saponins and ilexoside XXIX as indeices. to study the influence of different extraction factors such as extraction solvent, the volume of solvent, the extraction time and the frequency, and investigate the influences of the sample concentration, resin type, the largest absorption quantity, type and dosage of elution solvent to the macroporous resin refining technique. Secondly, Carried out antiviral model both in vitro and in vivo to have a primary efficacy evaluation of macroporous resin refining process. Thirdly, investigated the stability of ilicis asprellae liquor concentrated under different temperature(60℃,70℃, 80℃,100℃). Finally, compared three kinds of drying process to optimize the drying method.3 Pilot plant test research. Tracked pilot plant from extracting, refining, concentration to drying with retention ratio of total saponins and ilexoside XXIX as indeices. in order to verify the feasibility of the process parameters in pilot production. on the basis of the test in laboratory.4 Molding process research. According to the purpose of clinical treatment for acute paroxysm, the features of smaller viscosity after refined by the macroporous and bitter taste with little sweet. the formulation was confirmed as a buccal tablet, then selected different kinds of accessory to optimize the molding process.Results1 The subject established a TLC identification method and firstly built a content determination method of ilexoside XXIX with HPLC-ELSD. The result of the content determination showed that the content of ilexoside XXIX in root was higher than in stem, bark's was higher than xylem's, and the HPLC-ELSD chromatogram indicated that their constitutes were similar. ilexoside XXIX had not been detected in leaf. The result provided support for the use of the stem in the Guangdong province Chinese Medicinal Standard, and successfully improved the quality standard of ilex asprella.2 The preparation technology of total saponins from ilicis asprellae.. The results showed that the optimized technology was as follows:the crude drug extracted reflux 1.5h with 8 times of 60% ethanol, then repeated 1h with 6 times of 60% alcohol. The result of repeated experiment showed the retention rate of the total saponins and ilexoside XXIX were all reached 70%. the optimization of macroporous resin refining process was as follows: concentrated the ethanol from the extraction liquid thoroughly, then added water to dilute solution (1:5) to be absorbed by AB-8 macroporous adsorption resin column which had pretreatment (calculated by its absorption quantity of the total saponins,119.43 mg/g dry resin), then washed with distilled water until clarify, and eluted with 80% ethanol, collected three times column volumes of ethaol eluent. The repeated experiment with the optimized refining process showed that the retention of the total saponins and ilexoside XXIX were 83.71% and 89.46% respectively. The content of the total saponins and ilexoside XXIX in the outcome were 87.03% and 10.83%. the content indicated that the refining process can reach the technical requirements, and retain the effective parts, the process is rational and feasible. Results of primary efficacy evaluation of macroporous resin refining process and the total saponins showed that the antiviral efficacy of inhibiting the viral pneumonia in mice was retained before and after refining, and the total saponins outcome can restrain the 90% nose V14 when the concentration of the total saponins was 25mg/ml. the extraction before refining can show 5%-10% toxicity in the A549 when the concentration of the extraction from ilicis asprellae was 20mg/ml and also had certain RSV inhibition. The results of the stability of ilicis asprellae liquor concentrated under different temperature showed that after ilex asprella had been heated under different temperature (60℃,70℃, 80℃,100℃) for six hours, there was no significant influence on the content of total saponins and ilexoside XXIX, but the rate of total saponins was reduced sharply under 100℃. Combined with the production of equipment performance, the concentrated temperature should be adjust to less than 80℃. The results of drying process research showed that spray drying or decompression drying were optimized.3 The results of pilot plant test research indicated that the retention rates of the total saponins and ilexoside XXIX were 81% and 75% during the extracting process,91% of total saponins and all ilexoside XXIX were retained during the refining process.90% and 99% of total saponins and all ilexoside XXIX were retained during the concentration process.80% and 95% of total saponins and all ilexoside XXIX were retained in the drying process, finally the content in the outcome of total saponins were 92.7% and 8.4% respectively. The content indicate that preparation technology of the ilicis asprellae is scientific, feasible and can be used for production.4 According to the selection from different kinds of accessory, the molding process was as follows:mixed the powder, sucrose and aspartame in proportion of 1:10:0.15. the mixture was increased by equal degree, then stirred while adding the 10% PVP and 95% ethanol to make soft material, the soft material went through the griddle, dried in 50℃-55℃and sifted, finally the granule with a good mobility was obtained. and can be pressed into tablet by the rotary tablet machine with 0.5% agnesium stearate as lubricant. the pressure was 25KN. the filling depth was 10.6mm.ConclusionThe project improved the present quality standard of ilicis asprellae, optimized the preparation parameters of total saponins in ilicis asprellae and its preparation, and further conducted pilot plant test, the content of total saponins in ilicis asprellae can reach relevant technical requirement. the study provided supports for the development of ilicis asprellae.
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