Studies On Preparation Process And Quality Standard Of Xingyu Jiangtang Capsules

Part 1 Studies on Preparation Process of Xingyu Jiangtang CapsulesObjective:To select the optimum preparation process with the help of the Orthogonal test and HPLC,on the basis of the Chinese Pharmacopoeia 2010.Methods:Take the method of boiling parts of the crude drugs,and Crushing the others.Mix the concentrated liquid and the Crude drug powder,then dry and crush again to preparate to capsules.1 The crushing processIn order to avoid the loss of active components, giving full play to the effect,and after reading the reference literature,we determined the method that taking Part of Rhizoma Coptidis,all the rhubarb, part of Rhizoma Dioscoreae crushed into the medicine.2 The extracting processAccording to the function and usage of each drug,we determined to extract the other drugs. Based on the pre experiment, Using water as extracting solvent,the water ratio(A), extraction time(B) and extraction times(C) as factors, Each factor 3 levels, Using the table of L9(34) to make the orthogonal test. Making The rate of paste as evaluation index to select the best process.3 Determination of berberine hydrochlorideDissolve the Dry extract of 9 samples in the orthogonal test with Methanol 5ml to make 9 sample solution.Then put the standard into Methanol to make the solution of 0.5mg/ml as the standard solution. Measure the 9 sample solution and the standard solution 10μL respectively to inject liquid chromatograph to Analysis. Then we obtain chromatogram maps respectively, and compare them. With which we can verify the relationship between the dry extract and the contents of berberine hydrochloride.Results:1 Confirm the crushing process: Drying and Crushing 1/3 of Rhizoma Coptidis, all amount of rhubarb, 1/2 of Rhizoma Dioscoreae into powder through 60 mesh sieve.2 The Results of orthogonal test showed that the influence on the rate of plaster from large to small in turn is:the extracting times>the extracting time> The amount of water. The rate of dry paste between the sample of different extracting times(F=156.91) and the sample of different extracting time(F=38.22) is statistical difference;The sample of different amount of water and the rate of dry paste is not statistical difference(F=0.10).A further two two comparison by SNK method showed that the rate of dry paste of the sample extracting 2 times and the sample extracting 3 times is not statistical difference,but thay are both statistical difference with the sample extracting 1 time. The rate of dry paste of the sample extracting 1.5 hours and the sample extracting 2 hours is not statistical difference,but thay are both statistical difference with the sample extracting 1 hours. The rate of dry paste of the samples of different amount of water are not statistical difference. Thus we confirmed the extracting process is A(2,1)B(3,2)C(2).It is that extracting 2 times,first time 2 hours with 10 times water and second time 1.5 hours with 8 times water.Conclusions:1 Through the test,the best preparation process for Xingyu Jiangtang Capsule was determined: Drying and Crushing Part of Rhizoma Coptidis, all amount of rhubarb, part of Rhizoma Dioscoreae into powder through 60 mesh sieve.Put the remainder of the medicinal materials in the prescription into the Extraction pot. Decoction two times, the first boiled2 hours with 10 times amount of water and the second time boiled 1.5 hours with 8 times amount of water.Then mixed the liquid of two times, Filter it. Concentrated it to a relative density of about 1.25(90 ℃).Mixing the powder into,and drying.After which is Crushed into fine powder, into the hollow capsule.The method is stable and feasible. Part 2 Studies on Quality Standard of Xingyu Jiangtang CapsulesObjective : To establish the method of Identifying the TLC identification of Rhizoma Coptidis in prescription, rhubarb, Fructus aurantii Immaturus three medicinal herbs,and the determination method of the content of berberine hydrochloride in Rhizoma Coptidis.Methods: Identify the three batches of samples produced With the optimal preparation process by the following methods, and detecte them. 2.1 Identifying the Coptis chinensis, Chinese rhubarb, Fructus aurantii Immaturus by the TLC. 2.2 Determinate the content of berberine hydrochloride in the capsules by the HPLC. 2.3 Detecte the samples by the rules of preparations in accordance with the provisions of the Chinese Pharmacopoeia 2010 edition. The moisture detection,content uniformity,disintegration time,microbial limit test etc.Results:1 The results of Identifying the Coptis chinensis, Chinese rhubarb, Fructus aurantii Immaturus by the TLC is:Taking Butanol- Glacial acetic acid- Water(7:1:2) as developing agent, Coptis chinensis has clear spots under the UV lamp(365nm); Taking the The upper solution of Petroleum ether(30~60℃)- Ethyl formate- Formic acid(15:5:1) as developing agent, Chinese rhubarb has clear spots after smoked by Ammonia; Taking Ethyl acetate- Methanol-water(100:17:13) as developing agent, Fructus aurantii Immaturus has clear spots after air injected with aluminum chloride solution and placed after 2 hours.These chromatographic conditions have good reproducibility,and the negative sample have no interference.2 The chromatographic column of Hypersil ODS2 C18(250mm×4.6mm,5um) was used in the HPLC.In which the mobile phase is: Acetonitrile-Potassium dihydrogen phosphate(regulate the PH to 3 by Phosphate)(30:70).The temperature of the chromatographic column was 25℃,and Current Speed was 1ml/min. The wavelength is 345 nm.By which we measured the regression equation of Berberine hydrochloride is Y=71249X+84810, r=0.9995,it has A good linear relationship in 2.5-50 μg range.According to HPLC the measured sample content of 1.371%. The method is stable and feasible, high precision, good repeatability. 3 The moisture detection,content uniformity,disintegration time and the microbial limit test on the capsules were all confirm to the provisions of the general principles of the preparation in the Chinese Pharmacopoeia 2010 edition.Conclusions:1 The method of TLC built for the Coptis chinensis, Chinese rhubarb, Fructus aurantii Immaturus is Specificity.The spots are clear,which can accurately identify the preparation medicine.2 The HPLC is used for the determination of the content of berberine hydrochloride in the Xingyu Jiangtang Capsules.It has high accuracy, strong specificity, good reproducibility, can effectively control the quality of preparation.