Study On Preparation Technology And Quality Standard Of Anshen Granule

ObjectivesInsomnia is a common clinical refractory disease. The long-term poor sleep easily leads to premature aging, causing illness, such as depression, high blood. The original prescription of Anshen Granule is a clinical prescription, which is composed of Salviae Miltiorrhizae, Schisandrae Chinensis Fructus, Gastrodiae Rhizoma, Ophipogonis Radix and Lilli Bulbus, its efficacy is to support the liver and tranquilize. This study combined modern science and technology to optimize the preparation process, and undertake preliminary quality standard research.MethodsThe topic mainly contains three parts:extraction and purification process, forming process, three pilotscale experiment and quality standards of Anshen Granule.1. Extraction and purification technology research:According to material properties in the prescription, prescription was divided into two parts. Salviae Miltiorrhizae, Ophipogonis Radix and Lilli Bulbus use the method of water extract-alcohol precipitation. With salvianolic acid B (SalB) content and extraction rate as the index, through orthogonal test optimization to explore how solvent times, extraction duration and extraction times affect the water extraction, further determine the optimum conditions for extraction. With transfer rate of salvianolic acid B and ratio of extraction as review indicators, we used orthogonal test to explore relative density of liquids and ethanol concentration, which have influence on alcohol precipitation process. Then we screen a better purification process conditions. We use content of schizandrin and extraction rate as indicators, investigating how extraction duration, ethanol concentration and solvent times will have impact on the alcohol extraction process, and to have single-factor inspection of extraction times.2. Forming process research:This study determines to use dry granulation according to process results and practical situation. With the molding rate and moisture absorption as the index and refer to liquidity of granules, this study determine the impact of types of supplementary material, medicine auxiliary ratio and ethanol concentration on the molding process. Through the orthogonal experiment method, the study optimizes the best molding process.3. Quality standards research:In order to guarantee the quality of the granule, this carried out the routine examination and studied the quality standard from qualitative and quantitative aspects. This study identified Salviae Miltiorrhizae, Schisandrae Chinensis Fructus, Gastrodiae Rhizoma and Lilli Bulbus by TLC method and determined the content of salvianolic acid B and schizandrin by Using high performance liquid chromatography (HPLC) method, then established the quality standard initially.Results1. Extraction and purification process result:Water extraction process conditions:adding 12 times the amount of water, Bi hour’s heating reflux for 2 times.Alcohol sinking process conditions:The filtrate was concentrated to a relative density of 1.00-1.05 (60℃), the alcohol concentration of Ei and Placed for 24 hours.Alcohol extraction process conditions:adding 12 times of 85% alcohol, heating reflux 1 time for J3 hours.2. Forming process results:Wet granulation, Ki as excipients, drugs and excipients ratio is 1:1.5, M3 ethanol as wetting agent, environmental critical relative humidity at 70% or less.3. Establish quality standards:Set up the TLC qualitative identification method for Salviae Miltiorrhizae, Schisandrae Chinensis Fructus, Gastrodiae Rhizoma and Lilli Bulbus; the high performance liquid content determination method for salvianolic acid B and schizandrin. Chromatographc conditions for salvianolic acid B and schizandrin: Thermos SB-C18 (4.6mmx250mm,5μm) chromatographic column; mobile phase was acetonitrile-water, and the elution conditions was 0 to 10 min, (A) 20% to 25%,11 to 18 min, (A) 25% to 50%,19-35 min, (A) 50% to 80%,36 and 37 min, (A) 80% to 20%,38-40 min, (A) 20%, the flow rate of 1.0 ml/min, detection wavelength of 250 nm. And the content of salvianolic acid B and schizandrin in the Anshen Granule cannot be less than 3.01 mg/g and 0.39 mg/g, respectively.ConclusionBy analyzing the the preparation process of Anshen Granule, a stable and feasible molding process was established, and further produced qualified product. This study carried out qualitative identification and content determination as well, and set up quality standards to ensure the good quality of the granule.