Studys On The Preparation Technology And Quality Standards Of Yigen Tiaoli Paste

Objective: According to the requirements of the Registration of Pharmaceutical Preparations in Medical Institutions,to develop a Traditional Chinese Medicine paste named YiGen TiaoLi Paste for treatment of nocturia through mining the ancient prescriptions which is used to treat frequent micturition and nocturnal comes from Bencao Gangmu.Methods:(1)Study on extraction technology: Through orthogonal test,the adding amount of water,extraction time,number of repeated extractions were investigated,taking weighted comprehensive evaluation of polysaccharide content and yield of dry extract as an index,to determine the best extraction technology of Polygonatum kingianum Coll.et Hemsl.,Polygonatum odoratum(Mill.)Druce and Morus alba L.Through orthogonal test,volume fraction of ethanol,solvent,extraction time,number of repeated extractions were investigated,taking comprehensive evaluation of the content of flavonoids,Psoralen and Nootkatone as an index,to determine the best extraction technology of Rubus chingii Hu,Morus alba L.,Psoralea corylifolial L.,Alpinia oxyphylla Miq.,Allium tuberosum Rottl.ex Spreng.,Cannabis sativa L.and Crataegus pinnatifida Bge.(2)The study on preparation: Combined with response surface methodology with the weighted overall desirability(OD)value of the smell,liquidity,the taste and water content as an index,the effects of mixture adjuvant amount(A),the relative density of extract(B)and preparation time(C)were investigated by Box-Behnken design.(3)The study on quality standard: The qualitative identification of Polygonatum kingianum Coll.et Hemsl.,Alpinia oxyphylla Miq.,Psoralea corylifolial L.in Yigen Tiaoli paste were identified by TLC.Traits,relative density,insoluble and water content of Yigen Tiaoli paste were checked.The content of Psoralen and Nootkatone were determined by HPLC.(4)Preliminary study on stability: According to the Technical Guidelines for Stability Research of Traditional Chinese Medicine and Natural Drugs,the accelerated stability and long-term stability test of three batches of Yigen Tiaoli paste were investigated in accordance with the relevant regulations and the draft quality standard.Results:(1)The best water extraction process was: the herbs with water 10 times,two extraction cycles,each time for 1.5h.The best ethanol extraction process was: the herbs with 60% ethanol(12times),extracted 2 times,each time for 1.5h.(2)The best conditions in the preparation process of Yigen Tiaoli paste were as follows: the mixture adjuvant amount was 50%,the relative density of extract was 1.05-1.10 and Preparation time was 30 min.(3)Character research: Through the trait study of 3 batches of samples,the character of the Yigen Tiaoli paste was dark brown semi-fluid with uniform color and sweet scent;identification: through thin layer identification studies on 3 batches of samples,in the Polygonatum kingianum Coll.et Hemsl.and Alpinia oxyphylla Miq.In the thin layer identification test,the test sample chromatogram shows the spot of the same color in the corresponding position of the reference drug substance.The color is clear,the negative is not interfered,the separation effect is good,and the durability is good;in the thin layer of Psoralea corylifolial L.In the experiment,for the chromatogram of the test sample,the spot with the same color is displayed in the position corresponding to the reference substance,the color is clear,the negative is not interfered,the separation effect is good,and the durability is good;inspection: the results are checked by checking the 3 batches of samples.The relative density of the six batches of samples was determined to be 1.09 to 1.11.The moisture content of the six batches of samples was determined to be 22.37% to 23.11%.Determination of content: A method for the determination of psoralen in Yigen Tiaoli paste was established.The regression equation for psoralen was Y=6834930X+19895.5(r=0.9999),the linear range was 0.0985 to 0.985μg,and the average recovery was 100.1%(RSD was 2.03%).The determination of six batches of samples showed that the psoralen content was 0.83 to 0.85mg/g.A method for the determination of carotenol in Yigen Tiaoli paste was established.The regression equation for Nootkatone was Y.=1262220X+2114.40(r=0.9999),the linear range is 0.110 to 0.660 μg,and the average recovery rate is 99.86%(RSD is 1.78%).The determination of 6 batches of samples shows that the content of Nootkatone is 142.38 to 157.50 μg/g.The limit of the content of psoralen and Nootkatone were established.The content of psoralen should not be less than 0.68mg/g,the content of Nootkatone should not be lower than 120.04μg/g.(4)The long-term stability test and the accelerated stability test for 6 months showed no significant changes in the parameters of identification,examination and content determination.Conclusion: Through the study on preparation technology,quality standard and stability test of Yigen Tiaoli Paste,a preliminary study on the pre-pharmaceutical declaration of Yigen Tiaoli Paste was completed.