| In this paper,the standard decoction was prepared according to the decoction requirements of "Technical Requirements for Quality Control and Standard Formulation of Chinese Medicine Granules".The standard decoction was used as a quality control reference to study the extraction,concentration,drying and granulation processes of Schisandra chinensis Fructus formula granules.The quality standard of Schisandra chinensis Fructus formula granule was established.The correlation between the glass transition temperature and the content of the extract was investigated.The internal factors of sticking to the wall of Schisandra chinensis Fructus extract by spray drying were explained,to provide theoretical guidance for the preparation technology and quality standard of Schisandra chinensis Fructus formula granules.The main research contents and conclusions were as follows:1.Select 15 different batches of Schisandra chinensis Fructus medicinal materials from different sources,according to the decoction requirements in the "medical institutions Chinese medicine decoction room management practices",the standard decoction was prepared.Using the average±3SD algorithm,the transfer rate of schisandrol A in the standard decoctions was set to be 21.28%～33.85%,the extract yield was 31.90% to 38.91%,which provided reference for the subsequent quality control of Schisandra chinensis Fructus formula granules.Schisandrol A is a lignans with DMSO≥13mg/m L,soluble in chloroform,methanol,acetone,etc.,with low solubility in water.The standard decoction was extracted with water as solvent according to the clinical use habit,so the transfer rate of schisandrol A was low.2.Guided by the basic theories of traditional Chinese medicine,and based on the previous research,relevant experimental studies were carried out to optimize the extraction,drying and granulation process parameters of Schisandrae chinensis Fructus formula granules,providing a theoretical basis for the study of Schisandrae chinensis Fructus formula granules.L9(34)orthogonal table was selected to investigate the effects of water dosage,extraction time and extraction times on the extraction results,with the transfer rate of schisandrol A and extract yield as indexes.The optimal extraction process was optimized.The results showed that the extraction times was the most important factor,followed by the addition of water.The optimum extraction process of Schisandra chinensis Fructus was determined to be 3 times with 8 times of water for each time and decocting for 1hour.Under this condition,the index component transfer rate of Schisandra chinensis Fructus and the extract yield value were in the standard decoction index range.3.Spray drying of Schisandra chinensis Fructus extract was seriously sticky,while the drying process could not be carried out.Adding maltodextrin to the extract was helpful to improve the wall stickiness of the extract of Schisandra chinensis Fructus by spray drying and improve the powder yield.The effects of different DE values and added amounts of maltodextrin on spray drying of the extract of Schisandrae chinensis Fructus were compared.The physicochemical properties of the dried powder were determined.The process parameters of spray drying were optimized by using full factor experimental design.The optimum spray drying process conditions of Schisandra chinensis Fructus was determined as follows: the addition of maltodextrin(DE10)with a solids content of 40% in the extract solution,inlet air temperature of 140℃,liquid inlet speed of 7.5m L/min,atomization pressure of 45 mm Hg,compressed air ratio of 100%.The powder yield was70%,the critical relative humidity(CRH)of the dry powder was 49.43%,the bulk density was 0.30g/m L,the tapped density was 0.51g/m L,and the Angle of repose was 51.8°.4.The forming process of the formula granules was studied and the dry granulation method was finally selected.The effects of maltodextrin,dextrin and lactose on the dry granulation of Schisandrae chinensis Fructus extract powders were investigated to select the best proportion and optimize the process parameters of dry granulation.The process parameters were finally determined as follows: primary and auxiliary ratio was 1:1.5,that is,(extract powder 100g+40g maltodextrin):110g maltodextrin,roller pressure 2.0MPa,roller rotation speed 10 Hz,side seal pressure 2.0MPa.It could provide reference for the forming process of Schisandra chinensis Fructus formula granules.5.In the spray drying process of the extract of Schisandra chinensis Fructus,if no pharmaceutical excipient were added to help spray,the drying powder would sticky wall.Experiments have shown that small molecular substances such as organic acids and small sugars cause sticky walls,while large molecules such as proteins improve sticky walls.In the early stage,the research group introduced the concept of glass transition temperature(Tg)into spray drying.By adding appropriate auxiliary materials to improve the Tg value of the mixture,the spray drying could proceed smoothly.The contents components in 15 batches of water extract of Schisandra chinensis Fructus were determined,the protein content ranged from 22.77mg/g to 35.75mg/g,total phenol content ranged from 3.40mg/g to 4.92mg/g,the tannin content ranged from 1.58mg/g to 3.11 mg/g,fructose content ranged from 0.78mg/g to 5.23mg/g,glucose content ranged from 0.01mg/g to 3.82mg/g,the total polysaccharide content ranged from 7.37 mg/g to 17.68mg/g.And the correlation between the contents of components and the glass transition temperature(Tg)of the spray powder was analyzed,which provided a theoretical basis for the spray drying process of the Chinese medicinal materials extract which is easy to stick to the wall.6.In order to ensure the quality of its preparation,the characters,identification,inspection and content determination of functional index components of several batches of Schisandra chinensis Fructus formula granules were carried out according to the relevant quality standard requirements of China Pharmacopoeia(2015 edition)1 and 4parts.The results showed that all of them met the requirements of granules,and the average content of schisandrol A in the granules was2.33mg/g.The draft quality standard of Schisandra chinensis Fructus formula granules was prepared to provide reference for enterprises to formulate product standards.In this project,the raw materials of Schisandrae chinensis Fructus formula granules was used according to the concocted specifications,the extraction,concentration,drying,granulation and other processes of Schisandrae chinensis Fructus formula granules were studied scientifically and reasonably,and the experimental parameters were optimized,the correlation between the glass transition temperature of the extract of Schisandrae chinensis Fructus and the composition of the extract solution of Schisandrae chinensis Fructus was studied,which laid a foundation for the research and development of Schisandrae chinensis Fructus formulation granules rich in sugar. |
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