| AD-2 is a saponin obtained by hydrolysis of ginseng plant saponins,and has good anticancer activity.C20 is a chiral molecule with isomers.Isomers of different configurations,usually have different pharmacological,pharmacokinetic activity and toxicity and other biological properties,in order to further study the efficacy of differences.A method of reversed phase high performance liquid chromatogram-light scattering detector(RP-HPLC-ELSD)was developed to separate and prepare a large number of AD-2 epimeric mixture,in order to explore the best separation conditions between method of continuous sampling interval and off-line preparation method.The separation consequence of the method of continuous sampling interval and off-line preparation method were investigated respectively,under different proportion of mobile phase and concentration of sample volume,and to compare work efficiency and other attributes of the different preparation methods.The suitable operation conditions of the two methods and the result of the preparation were obtained:method of continuous sampling interval,the mobile phase is methanol and water(83:17,v/v),and the feed concentration and volume age is 20 mg/ml and 1 mL,respectively,while the flow rate is 20 ml/min,under above conditions the preparation efficiency of 20(S)-AD-2 and 20(R)-AD-2 is 18.01 and 35.36 mg/h,respectively;off-line preparation method,the mobile phase is methanol and water(81:19,v/v),and the feed concentration and volume age is 200 mg/mL and 2.5 mL,while the flow rate is 20 mL/min,The preparation efficiency of 20(S)-AD-2 and 20(R)-AD-2 is 50.55 and 51.93 mg/h,respectively.Preparation efficiency of off-line preparation method is higher than that of the method of continuous sampling interval,and this method is convenient and reliable and large amount of 20(S)-AD-2 and 20(R)-AD-2 can be prepared for the separation and preparation of AD-2 isomer establish a good foundation.AD-2 as a solid raw material drug,the majority of the body test process using solid drug route,solid drugs as a pharmacological action of the material,and other substances as there are different internal molecules arranged in the same polycrystalline,Including crystalline and amorphous.Drug crystal form will make different clinical use of pharmacological effects,affecting the efficacy of drugs and produce side effects,in addition to the existence of drug polymorphism will affect its stability and safety in the production and storage process will also change,In order to ensure the quality of drugs,the development of the most competitive drug crystal or amorphous form is the current drug research and development process important research content.In this study,the AD-2 polymorph was studied for the first time.Crystallization of the AD-2 polycrystal was carried out by cooling the volatilized crystals in a nearly hot saturated solution.Crystallization was carried out in an ethanol solvent to obtain an amorphous powder by vacuum drying in a reverse solvent And characterized by powder diffraction(PXRD),infrared spectroscopy(IR),electron microscopy(SEM)and differential thermal analysis(DSC),and the differences in the efficacy of crystal I and unformed powder mice were investigated.(KM)mice were randomly divided into blank control group(Con),model control group(CCl4),AD-2 crystalI group(CCl4+crystalI),Unshaped Powder group(CCl4 + Unshaped Powder)and positive control group(CCl4 + SFJ).The rats were treated with CCl4 for 7 weeks,After the last administration,the blood was taken from the eye,and the liver was examined.The therapeutic effect of AST,ALT and liver injury and fibrosis were compared.The results showed that both crystalline I and indefinite powder could decrease the levels of AST and ALT in the serum,reduce the inflammatory infiltration of the liver and the damage of the cells,reduce the proliferation of collagen fibers and the best treatment of amorphous powder... |
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