Study On Preparation Technology And Quality Standard Of Xieriga-4 Dropping Pills

Objective: To combine the advantages of traditional prescription of Mongolian medicine with modern new dosage form and preparation technology,to complete the preparation process and quality standard research of Xieriga-4 dropping pills,and to lay a foundation for the development and application of Xieriga-4.Methods: 1.The optimal extraction conditions of curcumin oil with supercritical CO2 were optimized by orthogonal test,with the oil yield and the peak area of curcumin under the condition of m/z119-120 as indexes.The single factor test and orthogonal test were used to optimize the process conditions of ethanol extraction of oil-free curcuma with curcumin and extract rate as indexes.Using gardenoside and berberine hydrochloride as indexes,the optimal extraction conditions of Tribulus terbulis,Gardenia jasminoides and Phellophellus chinensis were optimized by single factor test and orthogonal test.2.Using gardenoside and berberine hydrochloride as indexes,the single factor test and orthogonal test method were used to optimize the water extraction conditions of turmeric,tribulus terbulis,gardenia and Phellophellus chinensis.3.Curcuma powder was directly used as medicine.Using gardenoside and berberine hydrochloride as indexes,the single factor test and orthogonal test method were used to optimize the water extraction conditions of Tribulus terbulis,Gardenia jasminoides and Phellophellus chinensis. 4.Using the three extracts obtained from the above experiments as materials,single factor test and orthogonal test were adopted respectively,and the optimal forming conditions of Xieriga-4 dropping pills were optimized by taking the appearance quality,dispersion time and weight difference of dropping pills as indexes.The quantitative identification of curcumin and gardenoside in three kinds of Xieriga-4 dropping pills was carried out by HPLC.Results: 1.The optimal conditions of supercritical CO2 extraction were as follows: extraction pressure 30 MPa,extraction temperature 55℃,extraction time 1.5h.The optimum extraction conditions of turmeric were12 times of 75% ethanol,3 times of 1 hour each time.The optimum extraction conditions of Tribulus terrestris,Gardenia jasminoides and Pseudomonas chrysalis were 12 times water,5 times,0.5h each time.The optimum forming conditions of Xieriga-4 dropping pills were as follows:PEG4000:PEG6000=1:1 as matrix,the ratio of drug to matrix was 1:2,the coolant was dimethylsilicone oil 100,the liquid temperature was 80℃,the coolant temperature was gradient cooling(the upper temperature was39℃,the lower temperature was 5-10℃),the drop rate was 25 ～ 30d/min,and the drop distance was 10 cm.It was determined that Xieriga-4dropping pills were light brown pills with aroma and slightly bitter taste.The recovery of curcumin in dropping pills was 100.17%,and the RSD value was 0.54%.The contents of curcumin in three batches of samples were 13.63mg/g,13.58mg/g and 13.21mg/g,respectively.The recovery of gardenoside was 99.35% and the RSD value was 1.09 %.The contents of gardenoside in three batches of samples were 17.86mg/g,17.61mg/g and 17.81mg/g,respectively.The weight difference,dissolving and dispersive time limit and content determination of the three batches of dropping pills were all in line with the regulations of the Chinese Pharmacopoeia(2020 edition)on dropping pills.2.The optimal extraction conditions of turmeric,tribulus terrestris,gardenia and yellow cymbidium were as follows: 12 times of water was added to extract turmeric,tribulus terrestris,gardenia and yellow cymbidium with 1.5 hours each time.The optimum forming conditions of Xieriga-4 dropping pills were as follows: PEG4000:PEG6000=1:1 as the matrix,the ratio of drug to matrix was 1:2,and the liquid temperature was80℃.It was determined that Xieriga-4 dropping pills were dark brown pills with aroma and bitter taste.The recovery of gardenoside in dropping pills was 100.39%,and the RSD value was 1.06%.The contents of gardenoside in three batches of samples were 23.46mg/g,22.98mg/g and23.32mg/g,respectively.The weight difference,dissolving and dispersive time limit and content determination of the three batches of dropping pills were all in line with the regulations of the Chinese Pharmacopoeia(2020 edition)on dropping pills. 3.The optimum conditions for water extraction of turmeric powder,tribulus terrestris,gardenia and yellow cypressing were as follows: 12 times of water was added,5 times of extraction,0.5h each time.The optimum forming conditions of Xieriga-4 dropping pills were as follows:PEG4000:PEG6000=1:2 as the matrix,the ratio of drug to matrix was1:2,and the liquid temperature was 85℃.The recovery rate of curcumin in dropping pills was 100.08%,and the RSD value was 0.45%.The contents of curcumin in three batches of samples were 6.25mg/g,6.32mg/g and 6.26mg/g,respectively.The recovery of gardenoside was101.31% and the RSD value was 1.63%.The contents of gardenoside in three batches of samples were 0.88mg/g,0.87mg/g and 0.89mg/g,respectively.The weight difference,dissolving and dispersive time limit and content determination of the three batches of dropping pills were all in line with the regulations of the Chinese Pharmacopoeia(2020 edition)on dropping pills.Conclusions: The preparation process of three kinds of Xieriga-4dropping pills is simple,safe,stable and feasible.The quality standard is accurate and controllable,and the dropping pills have good stability,which lays a foundation for the production,application and further research of Xieriga-4 dropping pills.