| Objective: To re-evaluate the quality standard,extraction process and purification process of Qingnao Fushen Oral Liquid.Methods:1.In the study of quality standard,Aurantii Fructus,Puerariae Radix,Radix paeoniae Rubra were identified by TLC.The p H and relative density were determined according to Chinese pharmacopoeia(2015 Edition).The berberine hydrochloride and total flavonoids were determined through HPLC and UV-Vis.The evaluation methodology of Qingnaofushen oral liquid by UV-Vis and infrared fingerprints were established by using correlation-coefficient to calculate similarity.2.In the study of preparation process,the influence factors are the amount of solvent,the velocity of percolation and the concentration of ethanol.By selecting L9(34)orthogonal test design to achieve the optimum conditions of extraction process of percolation.The adsorption process of the activated carbon was used to pretreat oral liquid before purification process.The multi-factor parallel test was used to obtain the aperture,pressure,temperature and collection.To select the method of cleaning of membrane through the combination of different cleaners after purification process.3.In the study of the drug effects between two processes,to compare the drug effects before and after technical reforms through the number of mice fall asleep at the threshold dose of sodium,effects of sodium on sleep latency and hours of sleep,prolonging reaction time of mice pain threshold by heat stimulation as well as reducing the number of mice caused by acetic acid.4.In the study of stability,to compare the regular examination,content,UV-Vis spectrums,IR spectrums before and after cryopreservation of 10 batchs of Qingnaofushen oral liquid.Three batchs of Qingnaofushen oral liquid by the improved technology were normal temperature samples,and the preliminary stability of the samples were tested.Results: 1.The results of reevaluating quality standard were that: The TLC identification of Puerariae Radix,Aurantii Fructus,Radixpaeoniae Rubra were specific.Two good linear relationships were achieved over the concentration range of 0.03~2.10?g(r2=0.999)and 3.00~30.00?g(r2=0.999)for berberine hydrochloride and rutin.With two average recoveries of 101.03 % an d 9 8.51 %,RS D 1.16 %(n =6),2.24 %(n =6).Set the range of p H 4.66~7.00.The relative density may not be lower than1.00.And in the UV-Vis fingerprints,the similarity of the qualified samples was more than 0.993.In infrared fingerprints,the similarity of the qualified samples was more than 0.980.2.The results of re-evaluating preparation process were that: The percolation extraction process were solvent volume was 6 times of the weight of herbal medicine,the flow rate was10 m L·h-1(1.52 m L·min-1·kg-1),the concentration of ethanol was 40%.The adsorption process of activated carbon was as following: the usage of activated carbon of 0.1%,normal atmospheric temperature,adsorption time 20 minutes.The optimized process was: aperture 200 nm,pressure 0.10 Mpa,temperature 40?,collection 1.25 times of the original volume.The cleaning method of membrane is to use 1%Na OH to clean 30 minutes and 1% HNO3 to clean 30 minutes.3.The results of the drug effects between two processes were that: In sedative and hypnotic,compared with the original process,there was no significant difference between before and after technical reforms(P>0.05).It indicated that the improved technology had the same effects in cooperating with the hypnotic effect of pentobarbital and prolonging the hypnotic dosage of pentobarbital sleeping time.In pain relief,there was no significant difference between before and after technical reforms(P>0.05).It indicated that the improved technology had he same effects in prolonging reaction time of mice pain threshold by heat stimulation and reducing the times of twisting body caused by acetic acid.4.The results of the stability were that: The regular examination,berberine hydrochloride,IR spectrums before and after cryopreservation of 10 batchs of Qingnaofushen oral liquid were the same,but the total flavonoids and UV-Vis spectrums had changed.All the indexes of the three batchs of Qingnaofushen oral liquid were qualified in the first 12 monthes.Conclusions: This study revised the quality standard,the method is feasible,the limit is reasonable.It can be used as the standard for the quality control of Qingnaofushen oral liquid.After the improvement of the preparation process,the index components and the efficacy was equivalent with the original process,which indicated that the process was feasible and can be applied in the industrial production. |
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