| Objective:Xuanfeihuatan syrup is inconvenient for taking and carrying and easy to rancidity or precipitation. In addition, the sugar content of syrup is above 45% that can't meet the needs of diabetic patients. As a starting point, this experiment plan to change syrup into sugarless granules. Extraction, purification and molding process are optimized to formulate quality standard of this granules, which can provide theoretical data for mass production.Methods:1. Taking the peak area of amygdalin, ursolic acid, oleanolic acid and the whole party extract rate as index to determine the method of extraction.2. Taking laetrile transfer rate and the extract rate as the index, choosing L9 (34) orthogonal table to investigate extraction frequency, water addition and extraction time to confirm the best process of Xuanfeihuatan. Taking transfer rate and the extract rate of ursolic acid and oleanolic acid as indexes, select L9 (34) to investigate extraction frequency, extraction time, ethanol concentration and adding amount of ethanol to determine the optimal alcohol extraction process.3. Optimum centrifugal process can be determined by using the removal rate of impurity substance as index by probing into the effect of multiple factors including strength and temperature of solution, the time and rotation rate of centrifugation on the results of the experiment separately. Taking the removal rate as the target, alcohol precipitation process is optimized by orthogonal test of relative density, the amount of alcohol, and the alcohol precipitation time. In order to remove the impurity, single factor test is carried out to determine the content of chitosan, the concentration of liquid, and the temperature of flocculation. The optimum chitosan flocculation process is optimized by the orthogonal test of 3 factors and 3 levels. Comparing the optimum process of the above methods, the best impurity removing is determined.4. To determine the optimal concentration of the solution, the state of clear paste is observed. Quantity and state of the dry paste determine the proportion of dextrin. Dry method determined by comparing the drying efficiency and quality of different methods.5. With the yield of inclusion and inclusion rate as index, the proportion of menthol & beta CD, inclusion temperature, closure time are investigated to optimize inclusion process of menthol & beta CD.6. TLC & HPLC were used to study the qualitative and quantitative of enlarge test.Results:1. The best water extraction technology of the Xuanfeihuatan is that herbs first with 10 times amount of water, boiling 2 hours, than with 8 times amount of water, decocted for 1.5 hour. Decocting with 80% ethanol for2 hours is optimal alcohol extraction process.2. The optimum purification process is that liquid medicine is concentrated to containing crude drug 1g·ml-1, cooled to 30?, added to chitosan by 0.7 g·L1, stirring for 10 min, centrifugated 20 min by 5000 r·min-13. Based 1.35(50?) of density of the clear paste and the amount of added dextrin, the best drying method of the paste is microwave drying(75??) 45min than 30 min and 15min for 3 times.4. One mentholF& 10 times beta-CD in 60? for 4 h is the optimum inclusion process.5. The color and the position of main spots of the test sample is the same as it of the control article, and the negative is without interference on TLC.6. The chromatographic conditions of amygdalin is using methanol and 0.1% phosphoric acid solution (17:83) as mobile phase with octadecylsilane bonded silica as a filler. Theoretical plate number is not less than 5000 with the flow rate is 1 m·min-1 under 207 nm wavelength detection.The chromatographic conditions of ursolic acid and oleanolic acid is using acetonitrile methanol-0.5% ammonium acetate solution 67:12:21 with the flow rate of 1 ml·min-1 under 207 nm wavelength detection. Theoretical plate number is not less than 3000 with the same filler.Conclusion:The extraction, purification, concentration and drying process have be done and can be used for the mass production. TLC and HPLC can be used for the quality control. |
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