Study On The Process Optimization Of Dipsacus Asper Standard Decoction And The Quality Of Formula Granule

Dipsacus asper,the roots of Dipsacus asper Wall.ex Henry.With the drug efficacy of liver and kidney,strong bones,injury,metrorrhagia,tocolysis.It,s clinical actions are curing the pain in waist and leg bruises beriberoid disease metrorrhagia.The dipsacus asper formula granule are made from dipsacus asper pieces conforming to pharmacopoeia regulation and manufactured by modern technology of extract,concentration,spray drying and granulation.The advantages of dipsacus asper formula granule are taking convenient and storage.In order to guarantee the quality of dipsacus asper formula granule and to ensure the safety and effectiveness of its application,in this dissertation,studies on the technology of standard decoction and the process parameters were determined;determination the content of asperosaponin VI and paste rate of 10 batches of dipsacus asper standard decoction by the main technology are determined and the range of the content of asperosaponin VI and paste rate was established.The determination of the content of asperosaponin VI and the fingerprints from 10 batches of dipsacus asper formula granule and standard decoction by this technology.Dipsacus asper formula granule compared chromatograms with standard decoction.Objective: Determine the technology of standard decoction and determination the content of asperosaponin VI and paste rate of 10 batches of dipsacus asper standard decoction.The range of the content of asperosaponin VI and paste rate was established.To establish the method for determination of asperosaponin VI and fingerprint chromatogram.Dipsacus asper formula granule compared chromatograms with standard decoction,and to provide reference for the study of the quality and clinical application of the dipsacus asper formula granule.Methods:1 The content of asperosaponin VI and paste rate as the index.Extraction water volume,decoction time,decocting times as the investigation factors.Ten batches of dipsacus asper were prepared from representative samples through determine the final preparation technology by a process validation test,then determination the content of asperosaponin VI and the paste-forming rate.The range of variation of the paste-forming rate and the content of asperosaponin VI was specified by the standard deviation of 3 times the SD.2 The HPLC analysis determination of asperosaponin VI was carried out in Elite SinoChrom ODS-AP C18 column(4.6×150 mm,5?m)with a mobile phase of acetonitrile-water(30:70).The detection wavelength was set at 212nm;the flow rate was 1.0 mL/min;the column temperature was kept at 35 ?and the sample volume was 10?L.3 For 10 batches of dipsacus asper standard decoction and formula paticles of fingerprint are studied and compared the two reference chromatograms by UPLC.It was carried out in Waters ACQUITY UPLC BEH C18 column(2.1x100 mm,1.7?m)with a mobile phase of acetonitrile-0.1%phosphoric acid by gradient elution.The detection wavelength was set at 220nm;the flow rate was 0.3 mL/min;the column temperature was kept at 40 ?and the sample volume was 1?L.Results:1 The technology of optimum as follows: extract by The first boiling for13 times of water and soak for 30 min,high heat boil,micro soft fire keep boiling 60 min.extract by The second boiling for 11 times of water,high heat boil and micro soft fire keep boiling 40 min,filter immdiately with 100 mesh sieve and merge,then concentration under reduced pressure to extract solution with a relative density of 1.1(50?),finally,freeze drying into dry paste powder.In the standard decoction of dipsacus asper,the paste-forming rate was37.9%~42.7%,mean value of plus or minus 3 times SD to define the range of the rate for 36.5%~44.0%.the content of asperosaponin VI was42.04mg/g~62.54mg/g,mean value of plus or minus 3 times SD to define the range of the rate for 37.39mg/g~76.23mg/g.2 Asperosaponin VI were linear in the range of 0.4840 ~ 4.8400?g(r=0.9999).The average recovery of asperosaponin VI was 98.49%.The sample is stable within 24 h.The RSD of the repeatability was 1.13%.The content of asperosaponin VI was 59.89mg/g in dipsacus asper formula granule.3 The fingerprint chromatograms from 10 batches of dipsacus asper standard decoction and formula granules were established respectively.All the chromatograms possessed 17 same chrmatographic peaks in common.The four Components of Chlorogenic acid;Caffeic acid;Loganin;Asperosaponin VI were recognition by comparison with the standard chromatogram.The similarity of 10 batchs of dipsacus asper standard decoction was more than 0.9.The similarity of 10 batchs of dipsacus asper formula granules was more than0.95.Conclusions:The standard decoction process is stable and with good repeatability,the range of the paste-forming rate and the content of asperosaponin VI was reasonable,which can provide guidance for production formula granules particles.The method of determination content and fingerprint chromatograms in dipsacus asper formula granules is accurate,stable and with good repeatability.By comparing the dipsacus asper standard decoction and formula granules of the reference chromatograms,reflecting the formula granules and standard decoction are basically the same chemical composition,with quality consistency,which can provide reference for the study of the quality and clinical application of the dipsacus asper formula granule.