Studies On The Preparation Process And Quality Standard Of Paishi Granule

Liniao Paishi Granule is a new compound preparation of eight Chinese medicines, which consists of Lysimachia christinae Hance, Gallus gallus domesticus Brisson, Pyrrosia lingua(Thunb.)Farwell, Malva verticillata L., Curcuma wenyujin Y.H.Chen et C.Ling, Vaccaria segetalis(Neck.)Garcke, Clematis chinensis Osbeck and Glycyrrhiza uralensis Fisch. The prescription from the hospital is empirical and it has been used clinically for many years. It has the function of diuresis and preventing of urolithiasis. This study is about the extraction process, preparation process and quality standard of that prescritption. The propose is to ensure the preparation process is scientificly and establish the effective quality standard.In order to investigate the extraction process, dry extract rate and total flavonoids were used as the indecies, the single factor experiment about the solvent ratio, extraction time and extraction times were investigated. The results showed that the optimal extraction process of Liniao Paishi Granule is: extrating with 8 times with water for 3 times and 1.5 hour for each time, which is based on the L9(33) orthogonal design with 3 factors and 3 levels and considering the energy consumption, cost of production and other factors, we adjusted the extraction times to 2 times.The thesis carried out the ethanol precipitation for Liniao Paishi Granule, and found that the best ethanol concentration for precipitation was 50%. After that, we investigated in the preparation process such as the excipient, wetting agent and drying condition. And confirmed that the preparation process was 6g soluble starch as excipient, 75% ethanol as the wetting agent and dried at 70℃ for 2 hours. The finished angle of the granule was 29.5? and the granule was good to packaging.Through the pilot-scale experiment with 3 batches, which batch numbers were 201401, 201402 and 201403, respectively, we found that extraction process and preparation process were repeatable after the test of their particle size, water content, solubility and microbial number limit according to Chinese Pharmacopoeia(2010 edition).Then quality control experiments were carried out. We established the TLC methods to identify Curcuma wenyujin Y.H.Chen et C.Ling, Vaccaria segetalis(Neck.)Garcke and Glycyrrhiza uralensis Fisch. in Liniao Paishi Granule. The above developed TLC methods can employed as the quality standard of Liniao Paishi Granule.HPLC determination method of quercetin and kaempferol in Liniao Paishi Granule were finally developed in this thesis. With methanol-0.4% phosphoric acid(40:60) as mobile phase at flow rate of 1ml/min at 25°C, the samples were anlyzed and detected at 360 nm,. The result showed that quercetin and kaempferol had a good linear relationship between the concentration and peak area among 10.02~100.2μg·m L-1 and 10.04~100.4μg·m L-1. The regression equation of quercetin and kaempferol were A=44428c+1027 and A=42458c+632, r=0.9999. The average recovery of quercetin and kaempferol were 100.3%(n=6) and 99.9%, RSD were 0.8% and 0.8%;. The HPLC determination method of quercetin and kaempferol, accurate, sensitive and good reproducible, could be used for the determination of quercetin and kaempferol in Liniao Paishi Granule.