Process And Quality Study Of Compound Banlangen Liyan Granules Based On Specific Chromatograms Technology

Object:In order to improve the quality control and standards of Compound Banlangen Liyan Granules,which is short as Liyan Granules in the following,including Isatidis Radix、Scrophulariae Radix、Platycodonis Radix、Glycyrrhizae Radix,etc.The paper aims to use HPLC method to establish specific chromatograms and analyze 6 effective components in the Liyan Granules water extract.It was used to optimize the preparation process parameters,evaluate the key process and improve the quality of traditional Chinese medicine preparation process.Methods:1.Use the HPLC method to determinate the 6 effective contents(including adenosine,(R,S)-goitrin,liquiritin,angoroside C,harpagoside,glycyrrhizic acid)of the Liyan Granules water extract(referred to as the water extract in the following).2.In the same HPLC conditions,demarcate the common peaks of 10 batches of the water extract,and calculate the relative retention time and relative peak areas of common peaks.Use the chromatographic fingerprint evaluation system software(2004A version)to evaluate the similarity and establish the HPLC specific chromatograms of the water extract.3.Based on the previous research,with the transfer rate of the 6 effective components and the similarity of characteristics as the main index,respectively,optimize the water extract concentration of ceramic membrane microfiltration process,drying conditions of the extract and the grain.4.Evaluate the pilot process of Liyan Granules on the base of the loss rate of the 6 effective components and the specific chromatograms.5.Establish TLC identification methods of the 4 decoction pieces and an HPLC method of simultaneously determining the 6 effective contents.Inspect the Liyan Granules according to the 2015 edition of "Chinese Pharmacopoeia" granules"inspection" requirements for.Results:1.The HPLC method can be used to determine the content of the 6 components in the water extract.The separation degree,linear relationship,precision,stability,repeatability and the recovery rate of the sample are good.2.Estabilished the HPLC specific chromatograms of the water extract,demarcated the 19 common peaks with(R,S)-goitrin as the reference peak,there were good similarities with the standard specific chromatogram and with their similarity coefficients no less than 0.914.1～19 common peaks relative retention time are defined as:0.199,0.255,0.261,0.319,0.375,0.435,1.000,2.098,2.122,2.164,2.181,2.224,2.507,2.641,2.806,3.394,3.929,4.002,4.080.3.The optimal processes:the membrane separation solution concentration was containing crude drug 0.2 g/mL;drying condition of extract with the vacuum degree is-0.085 MPa～-0.095 MPa,60℃;70 0C with atmospheric pressure for the granules.4.Pilot process of Liyan Granules showed that there were differences in the single loss rate and the total loss rate of the 6 effective components in the 4 key processes within the same batch,extractors vacuum concentration and vacuum drying were the main processes of the 6 effective component loss,(R,S)-goitrin and harpagoside loss rate were higher than the rest 4,the similarity of HPLC specific chromatogram decreased with the increase of the number of processes;total losses of the 6 effective components in the 4 key processes were 48.15%and 50.85%,respectively,the overall HPLC specific chromatograms similarity of the pilot process of the 2 batches was good.5.The methods of TLC identification of the 4 decoction pieces and simultaneously determining the 6 effective contents by HPLC were feasible,which measured out the limit of contents.All inspection items were in compliance with the requirements of the 2015 edition of Chinese Pharmacopoeia.Conclusion:The method of the 6 effective contents and HPLC specific chromatograms in water extract of Liyan Granules established in one chromatograms is simple and scientific.The optimized preparation process is reasonable and stable.The HPLC specific chromatograms similarity of the 10 batches of the water extract shows good.It will improve the quality of Chinese medicine preparation process and quality standards and provide the basis for new drug research.