Improvements On Preparation Technology Of Qingwenjiedu Oral Liquid

Qingwen jiedu oral liquid,one of most common used compounded Chinese traditional veterinary preparations for prevention and control of poultry diseases recently,has the efficacy of clearing heat and toxic materials,mainly treating exogenous fever of poultry.But there are lots of deficiencies in traditional production,such as low extraction rates of active components,great losses in concentration and purification,as well as high energy consumption.In addition,there are only standards of qualitative identification for qingwen jiedu oral liquid but lack of standards of quantitative determination for mainly active components in the national quality standards,which could make influence on the stability control for the production quality and lead to low clinical efficacy of the oral liquid.For the problems mentioned above,the HPCL methodology for assaying of baicalin in qingwen jiedu oral liquid was established in the present study,which could supplyment the national standards at some degree.By using new technologies including membrane separation and enzymolysis,the recovery rate of active components in the oral liquid was leveled up,resource consumption was reduced and production cost was saved,as well as the product quality was elevated and the price was lowered by improving preparation technology.The detailed results of the research are as follows:(1)Establishment of the HPLC methodology for assaying baicalinbased on the original quality standards of Qingwen jiedu oral liquid in "compilation of national standards for veterinary drugs---the upgrade of veterinary drug standards from local level to national level",the HPLC methodology for assaying baicalin was established.The results showed the optimized HPLC conditions for Baicalin as followed.The samples were dissolved with 50%MeOH,disposed by ultrasound for 20 min(100w,40KHz),diluted by 50%MeOH,then metered by volumn,and finally filtrated by 0.45μm millipore filter.The HPLC trials were performed by Kromasil C18(250mm*4.6mm,5μm)with the mobile phase of MeCN:0.2%HPO4(22:78)at the rate of 1.0 ml/min,and detected at 274nm,40°C with 10μL loading volume.The HPLC results showed that the method has great RSD,accuracy,repeatability and high recovery,and can be used for quantitative determination of Baicalin.(2)Study on the crushing extraction techniqueThe crushing preprocess of herbal materials for prepartion of qingwen jiedu oral liquid were investigated and the influence of crushing extration on the recovery rate of active components was analysed,which proved the optimum conditions as followed:The materials were smashed and filtrated through 24 mesh sieve,added with eight-time volume of water and extracted for 50min at 90 °C.(3)Study on the enzymolysis techniqueIn advantage of high efficiency and specificity of enzymes,four kinds of enzymes of cellulase,hemicellulase,pectinase and amylase were selected according to characteristics of materials used for the oral liquid and made into the complex enzyme.After experiments,the dosage and the appropriate conditions for reaction of the complex enzyme were acquired as followed:0.1%for the optimum dosage;1:1:2.5:2 for cellulase:hemicellulase:pectinase:amylase;ph4.5;50 min for reaction,at 45 °C.(4)Study on the membrane filtration techniqueBy the selective fluid separation of ceramic membranes for Chinese herbal extraction,the influencing factors,including the pore size of membranes and temperature as well as pressure,were optimized for selective separation of active components from the extraction,achieving the goal of purification.The results showed that the optimizing conditions for filtration as followed:0.6μm ceramic membranes at 30°C,0.2Mpa.(5)Study on the membrane concentration techniqueThe oral liquid is concentrated at low temperature by ultrafiltration membranes.Orthogonal experiments were designed and conducted for optimization of parameters such as pressure,temperature,membrane flux and membrane pollution.The results showed that the steam efficiency is obviously higher than the traditional counterpart at the flow rate of 35.67 m/s,at 40°C,0.2Mpa.(6)Analysis of the pilot scale production by the new techniquesAfter a series of research for procedures of extraction and purification as well as concentration,all the new techniques were applied for the preparation of Qingwen jiedu oral liquid,and validated by pilot scale production to confirm its feasibility and stability.Results showed that by combination of new technologies,the yield of active components was apparently larger than before.Through acceleration tests for 6 months,the products meet quality specifications of characteristics,identification,content and microbial limitation,which confirmed that by new technologies the quality of qingwen jiedu oral liquid was stable.The products from the pilot scale production are qualified for the examination by Henan Institute of Veterinary Drugs Control.The research achievements are placed second in the scientific and technological progress awards by zhengzhou city and being applied for the national invention patent grant.The new preparation technology can evidently increase the yield of active components in the oral liquid and reduce the consumption of resource,save the cost of production,and better the quality of products.