Preparing Technology And Quality Control Of Qidan Granules

Qidan Granules is a compound preparation which is composed of nine herbalmedicines, and they are Astragalus, Salvia Miltiorrhiza, Panax Notoginseng, FriedAtractylodes, Dried Rehmannia Root, Fructus Corni, Rhizoma Anemarrhenae,Rhizoma Chuanxiong and Barbary Wolfberry Fruit. It is mainly applied for theadjuvant treatment of typeⅡdiabetes. In order to provide experimental basis for drugdevelopment, this subject has done systematic experimental studies on preparation,quality standards and preliminary stability according to the traditional Chinesemedicine theory and modern pharmaceutical technology.Study on preparationVolatile oil extraction study: Using steam distillation method to extract RhizomaChuanxiong volatile oil. Volatile oil extraction study selected extracted volatile oilvolume as investigation index, selected solvent amount and extract time as two studyfactors. It conducted single factor experiments and found out the optimal condition ofvolatile oil extraction. The optimal condition for volatile oil extraction study isextracting for8hours with the amount of10times water.Water extraction study: Using decocting method to extract herbal medicines.Water extraction study selected dry extract yield and AstragalosideⅣ content asinvestigation indexes, selected solvent amount, decocting time and decoctingfrequency as three study factors. It conducted L9(34) orthogonal experiments to findout the optimal condition of water extraction study. It also considered some practicalfactors such as energy saving, water saving and shortening the production cycle to getthe final decision. The optimal condition for water extraction study is boiling threetimes with the amount of10times water each time, and boiling for1hour each time.Refining process study: Using alcohol precipitation refining method to purify thewater extract. Refining process study selected dry extract yield and AstragalosideⅣcontent as investigation indexes, selected relative density of extractum, concentrationof alcohol precipitation and settling time as three study factors. It conducted L9(34) orthogonal experiments to find out the optimal condition of refining process study. Italso considered principle of energy-saving and emission reduction and practicality ofindustrial production to get the final decision. The optimal condition for refiningprocess study is adding alcohol to extractum (relative density is1.08) till alcoholconcentration reached50%and settling for12hours.Moulding techniques study: Using spray-drying granulation method to mouldQidan Granules. Moulding techniques study selected qualified particle yield andmoisture content as investigation indexes, selected the inlet velocity of liquid,atomizing pressure and the inlet air temperature as three study factors. It conductedL9(34) orthogonal experiments to find out the optimal condition of mouldingtechniques study. The optimum conditions for moulding techniques study is the inletliquid flows10mL/min with the2.4Pa atomizing pressure, and220℃inlet airtemperature.Study on quality standardUsing TLC method to identify Salvia Miltiorrhiza, Panax Notoginseng, FriedAtractylodes, and Fructus Corni in Qidan granules. The result shows that the testsamples share the same spot at the same position with reference sample and(or)control medicine both in size and color in each TLC plates. However, there is no spotat the same position in negative sample solution in every TLC plates.Using high performance liquid chromatography-evaporative light scatteringdetector(HPLC-ELSD) method to measure AstragalosideⅣcontent in Qidan granules.This study found out the optimum chromatographic conditions. Under this optimumchromatographic conditions, AstragalosideⅣ showed good linear relationship withina range of0.852-4.26μg; precision meets Pharmacopoeia requirements; averagerecovery of AstragalosideⅣ was97.55%, RSD=1.83%(n=6); RSD of AstragalosideⅣcontent determination of t hree batches of Qidan granules was0.23%.Detecting four test items of granules inspection items, and they are moisture,particle size, melting ability and loading differences. We did these tests to threebatches of Qidan granules and the results showed that every test items are in line withthe2010edition of Chinese Pharmacopoeia requirements for granules.Study on preliminary stabilityIn order to preliminary investigate stability and validity of Qidan granules, we conducted stability study in room condition test for6months and stability study inacceleration test for3months. The results indicate that all investigation indexes (TLCidentification of Salvia Miltiorrhiza, Panax Notoginseng, Fried Atractylodes, andFructus Corni; content of AstragalosideⅣ; moisture, particle size, melting ability andloading differences of Qidan granules)comply with the requirement, showing goodstability. Consequently, the validity period is presumed to be18months.