Study On Preparation Technology And Quality Standard Of Zhideke Granules

Objective:(1)The extraction technology of volatile oil and water was optimized for zhideke granules.The alcohol precipitation process,concentration process and drying process were studied.(2)The processing technology of zhideke granules was screened and the preparation technology was determined.(3)A draft quality standard for zhideke granules was established.Methods:(1)The optimμm extraction process was optimized by single factor and orthogonal test with the content of corresponding components as the index.The alcohol precipitation process,concentration process and drying process of water extract were investigated,and the process range was determined.(2)The optimμm preparation process of inclusion compound was obtained by orthogonal test with inclusion rate as the index.With soluble starch,dextrin,mannitol,microcrystalline cellulose and white sugar as auxiliary materials,the molding rate,Angle of repose,hygroscopicity and melting rate as indicators,weight method was used to score,and the best molding process was selected,Three batches of amplification process experiments were carried out.(3)Three batches of zhideke pilot-scale granules were studied by TLC,physical examination and content determination.Results:(1)Optimal extraction conditions of volatile oil: soak for10 min,add 4 times the amount of water,and extract for 3h;Optimal water extraction process conditions: add 12 times the amount of water,extract 3 times per copy,and extract for 90 min each time.Process parameters: use static method to remove impurity;Thick paste with a relative density between 1.25 and 1.35 is more suitable for particle production.Atmospheric concentration temperature range is 90 ～ 100℃;The scope of reduced pressure concentration conditions for 60 ～ 90℃and 0.04 ～ 0.09 mpa.Atmospheric pressure drying temperature range is80 ～ 100℃.Decompression drying temperature and vacuμm degree range is 70 ～ 90 ℃ and 0.05 ～ 0.09 Mpa.(2)The best rate of volatile oil inclusion process conditions: material ratio of 8:1,temperature 50 ℃,1 h stirring;The best type and ratio of admixtures was dextrin: white sugar=2:1,and the relative critical relative hμmidity of the particles was 77%.(3)On the TLC graph,the characteristic spots of the eight medicinal materials could be identified.The tested solution and the control medicinal materials showed the same color,and the spots were clear,while the negative control samples had no interference.Three batches of pilot test particle inspection items are qualified.In the content determination of irisin,the peak area and concentration of irisin in the range of 2.8000～ 42.0000 g/m L showed a good linear relationship,and the correlation coefficient was 0.99964;The sample recovery ranged from95 to 105%,and the RSD value was 2.05%,indicating that the results were reliable;The RSD values of the reproducibility and stability of zhideke granules were 1.85% and 2.49% respectively,indicating that the reproducibility and stability of the samples were good.In the content determination of baicalin,the peak area showed a good linear relationship with its concentration within the range of 0.0152～ 0.2280mg/m L,and the correlation coefficient was 0.99989;The sample recovery ranged from 95 to 105%,and the RSD was 2.06%,indicating that the results were reliable;The RSD values of reproducibility and stability of zhideke granules were 0.46% and 0.28%,respectively,indicating that the samples had good reproducibility and stability.In the content determination of total flavonoids,the absorbance of rutin reference substance showed a good linear relationship with the concentration within the content range of 0.1940～0.7760 mg,the correlation coefficient was 0.99983,the recovery of the sample was between 95 ～ 105%,and the RSD value was2.06%,indicating that the results were reliable.Conclusion: The optimμm conditions for extracting volatile oil and water from zhideke granule were obtained,and the parameters of concentration and drying processes were investigated,which provided a feasible experimental basis for the further development of zhideke granule.The optimμm technological conditions of inclusion compound and the proportion of auxiliary materials in the molding process were studied.The method was simple and feasible.Three batches of zhidake granules were obtained through the amplification process of zhidake granules in three batches,which played a guiding role in the standardized production of zhidake granules.The TLC method was used to identify eight kinds of Chinese medicinal materials with simple operation and clear spots.The results of particle size,water content,drying and weight loss,solubility and loading of granules were all in line with the standards of "granules" of the four general principles of the Chinese pharmacopoeia(2015).HPLC method was used to determine the average content of irisin in three batches of zhideke granules was 40.0736 ug/g,and the average content of baicalin was 4.8886mg/g.The average content of total flavonoids in zhideke granules was 13.0637mg/g by UV-Vis spectrophotometry.The method has the advantages of high speed,high sensitivity and good stability.