Study On The Preparation Technology And Quality Standard Of Qishen Granules

ObjectiveThe Qishen granule,which is composed of Astragalus mongholicus,Salvia miltiorrhiza,Flos Lonicerae etc,has the the curative effect of benefiting qi for activating blood circulation and resolving toxin for protecting the heart.It is used primarily to treat cardiac dysfunction in heart failure.The Qishen granule is formulated under the guidance of clinical experience of Prof.Wangwei's research group,and had many disadvantages about lot of respects such carry,storage and taking.So we study the extraction and purification of the compound Chinese medicinal preparation to make into granule by modern technology,in order to develop clinical effect,adapt to the need of market and provide high quality product for the patients.MethodFirstly,granules and water extracting-alcohol precipitating were selected by virtue of theories of pharmaceutical technology design and the characteristics of ingredients.The orthogonal was used to optimize decocting frequency,adding volume,extraction time by the content of Astragaloside IV,salvianolic acid B and paste-forming rate.In order to gain the best parameters of alcohol-precipitation procedure,we have inspected single factor influence on relative density,the volume of alcohol,time by the effective components and other apparent characteristics.Secondly,by comparing the dry granulation and wet granulation,we adopt the appropriate techniques.Then according to the date about moisture rate and angle of repose,we optimize the type and dosage of excipient.Furthermore,the CRH of Qishen granule has been measured to provide a reference for regulating environment condition.Lastly,we focus on the identification,determination and test of toxic component to control the preparation quality in the research.ResultThe optimum extraction condition of Qishen granule:A3B1C3,8 volumes of water,1 hour,3 times.The optimum alcohol-precipitation procedure:the solution was concentrated to the relative density of 1.10?1.15(60?)and precipitated with the alcohol concentration of 70%,then left to rest for 16 hours,centrifugal separation and drying under vacuum(60 ?,-0.8MPa).The shaping process:according to the proportion of 2:1,combined dry extract and lactose well,dry granulation,with roller speed 15 Hz and roller pressure 4MPa.The result of quality standard research:we have established the TLC method of Astragalus mongholicus and other four elements,as well as set up the HPLC method which is used to measurethe content of Astragaloside IV,salvianolic acid B and chlorogenic acid.Considerate the security aspect,a limiting detection for aconitine in the Qishengranule was also established as a TLC method.The chromatographic condition of Astragaloside IV:Apollo C18(4.6mmx 150mm,5?m),CH3CN-H2O(32:68),30?(column temperature),1.OmL/min(velocity of mobile phase),105?(drift tube temperature),N2,2.6mL/min(velocity of N2).The chromatographic condition of salvianolic acid B:AgilentTC-Ci8(4.6mmx250mm,5?m),CH3OH-CH3CN-HCOOH-H2O(27:10:1:62),30?(column temperature),1.0mL/min(velocity of mobile phase),286nm(UV detection wavelength).The chromatographic condition of chlorogenic acid:AgilentTC-Ci8(4.6mmx250mm,5?m),CH3CN-0.2%H3PO4(10:90),30?(column temperature),1.0mL/min(velocity of mobile phase),327nm(UV detection wavelength).ConclusionA stable and feasible preparation process of Qishen granule is established by the research of extraction,purification and moulding process,with producing qualified granules.The study had established criteria of qualitative identification,limit test and determination by the research of quality standards to provide a strong guarantee for preparation quality.In conclusion,the corollary of the experiment has reached the anticipant goal.