Study On Quality Standard Of Fufang Huangshen Granules

Compound Huangshen Decoction is an empirical prescription composed by old Chinese medicine practitioners for the clinical symptoms of chronic renal failure(CRF)following the principle of "syndrome differentiation and treatment".,The effect of purging turbidity,removing blood stasis,and benefiting water.This prescription has been used in the treatment of CRF in Chinese medicine for many years and has achieved satisfactory results.A good curative effect depends on the consistency of medication.Therefore,referring to the "Classification of Traditional Chinese Medicine Registration and Application Document Requirements" and "Measures for the Administration of Preparation Registration in Medical Institutions",it is proposed to make Compound Huangshen Decoction into granules to ensure its stable and reliable quality control.[Method]1.According to the 2020 edition of "Chinese Pharmacopoeia" and the 2011 edition of "Guangxi Zhuang Autonomous Region Drug Quality Standards(Volume II)" under the provisions of each prescription decoction piece,the prescription decoction pieces(astragalus,kidney tea,cooked rhubarb,epimedium Huobi and Licorice)were inspected separately,and the determination method of rosmarinic acid in kidney tea was established,in order to provide qualified decoction pieces for the preparation and quality standard research of compound Huangshen granules.2.On the basis of the extraction process of Compound Huangshen Decoction(completed by the cooperative research group),the HPLC fingerprints of the extract and its intermediates obtained by four drying methods were established,and the similarity analysis was carried out to obtain the compound Huangshen Decoction.Kidney granule intermediate preparation to determine optimal drying method.3.Research on the quality standard of 3 batches of compound Huangshen Granule intermediates(prepared by the cooperative research group): use TLC for qualitative identification,use HPLC fingerprint method for semi-quantitative research,and use HPLC method for content determination.Huangshen Granule quality standard research provides the basis.4.In order to ensure the quality uniformity of Compound Huangshen Granules in the later stage,this paper established a method for the simultaneous determination of12 components in the intermediates of Compound Huangshen Granules based on twodimensional liquid phase technology.5.Referring to the 2020 edition of the "Chinese Pharmacopoeia" Four General Rules 0104 granule items and intermediate quality standards,3 batches of compound Huangshen granule pilot test products(provided by the cooperative research group)were subjected to traits and inspections,TLC identification,fingerprints and In the content determination test,the quality standard of Fufang Huangshen Granules was comprehensively considered to ensure the stable quality of the drug.6.In order to investigate the quality stability of Compound Huangshen Granules,determine the drug packaging,storage conditions,and product expiration date,the stability test of Compound Huangshen Granules was carried out according to the relevant guidelines.[Result]1.In accordance with the relevant regulations in the 2020 edition of "Chinese Pharmacopoeia" and the 2011 edition of "Quality Standards for Drugs of the Guangxi Zhuang Autonomous Region(Volume II)",6 batches of Astragalus membranaceus,3batches of kidney tea,3 batches of cooked rhubarb,7 batches of epimedium,Three batches of licorice were inspected for quality,and the qualified decoction pieces were screened out for the preparation of compound Huangshen granules.2.The similarities between the samples under the four drying methods and the water decoction are all greater than 0.97,among which the spray-dried powder has the highest similarity.3.Established a TLC identification method for astragalus,kidney tea,licorice and cooked rhubarb decoction pieces in compound Huangshen granule intermediates,which is simple and reliable;The established fingerprint analysis method of compound Huangshen granule intermediates has good precision,stability and repeatability,and 35 common peaks can initially reflect the composition of the prescription of compound Huangshen decoction.The similarity between the 3 batches of compound Huangshen granule intermediates and the control spectrum was greater than 0.97,and at the same time,12 chromatographic peaks in the fingerprints of compound Huangshen granule intermediates,including calycosin glucoside,were identified;The established method for the determination of icariin,anthraquinones,and astragaloside in the intermediate of compound Huangshen granules is simple and feasible,and the content of each methodological investigation is in compliance with the regulations.The icariin content of 3 batches of compound Huangshen granule intermediates ranged from 1.33mg/g to 1.55mg/g,and the average transfer rate from decoction pieces to intermediates was 64.42%;the content of anthraquinones ranged from 3.33mg/g to 4.21 mg/g,the transfer rate from decoction pieces to intermediates is53.78%: the content of astragaloside IV ranges from 0.42mg/g to 0.50mg/g,and the transfer rate from decoction pieces to intermediates is 56.82%.4.Simultaneous determination of calycosin glucoside,epimedin B,liquiritin,rosmarinic acid,epimedin C,glycyrrhizic acid,aloe-emodin,rhein,epimedin A,The contents of 12 components including emodin,chrysophanol and icariin were well validated by the methodology;5.A set of draft quality standards for Compound Huangshen Granules was formulated,and the 3 batches of pilot test products of Compound Huangshen Granules all met the requirements after inspection;6.The properties,identification,microbial limit inspection and content of Compound Huangshen Granules simulated on the market did not change significantly during the test period,and all met the standards,indicating that the quality of Compound Huangshen Granules was stable under the test conditions;[In conclusion]In this paper,by using modern chromatographic analysis and two-dimensional liquid phase technology to study the quality standards of compound Huangshen granules intermediates,it is determined that the best drying method for the preparation of compound Huangshen granules intermediates is spray drying,and four TLCs of medicinal flavors are established.Chromatography,HPLC fingerprints,and content determination methods are reliable,and can be used for the quality research of compound Huangshen granules intermediates,and provide a method basis for the follow-up homogenization research of Compound Huangshen granules from the perspective of chemical composition;It complies with the feeding regulations and the quality is relatively uniform and stable.The quality standard of the finally established Compound Huangshen Granules is scientific and reasonable;the quality of Compound Huangshen Granules simulated in the commercially available packaging is stable under the stability test conditions and during the test period.