Study On Quality Standard Improvement Of Siji Sanhuang Pills

Siji Sanhuang pill has the effect of anti-inflammatory,antipyretic and convenient water circulation.It is made of four kinds of herbs,namely Phellodendri Chinensis Cortex,Rhei Radix Et Rhizoma,Gardenia Fructus and Scutellaria Radix.It is used for sore in mouth and nose,constipation in stool,red yellow in urine and other diseases.It has good curative effect on the disease of excess heat and fire poison.It is also recognized by doctors and patients in clinic and has high research value.The existing executive standard of Siji Sanhuang pills lacks the necessary items of identification and content determination,which can not control the quality of finished products.Therefore,it is necessary to improve the standard and establish a more perfect and reasonable quality control system.In recent years,the research of Siji Sanhuang pills mainly focuses on the content determination of individual chemical components(Rhei Radix Et Rhizoma),but other components in the four drugs also play a crucial role in the efficacy of the preparation.However,in the quality control of Siji Sanhuang pills,these researches are still one-sided,so it is necessary to improve the quality control level,Objective to provide reference for the internal quality control and evaluation of Siji Sanhuang pills.In this paper,the chemical components and blood intake components of the preparation were studied by UPLC-Q-TOF-MS/MS.The rapid analysis of chemical and blood components in sisisanhuang pills provides reference for the quality control and pharmacodynamics research.On this basis,by increasing quality control index,establishing fingerprint,we can draw up a more comprehensive quality evaluation standard of sisisisanhuang pill.The details are as follows:1.Study on the chemical constituents and blood constituents of Siji Sanhuang pills(1)Chemical composition study:UPLC-Q-TOF-MS/MS technology was used to qualitatively characterize the chemical constituents of Siji Sanhuang pills.The possible excimer ion peaks were speculated from the first-order mass spectrum.Combined with the secondary fragment ion information and self built database,76 compounds were found,including 12 anthraquinones,15 alkaloids,34 flavonoids and 15 terpenes,15 compounds have been compared with the reference substance.(2)Study on blood component spectrum:UPLC-Q-TOF-MS/MS technology was used to qualitatively analyze the plasma samples of rats after oral administration of Siji Sanhuang pills.By comparing with blank sample,preparation sample and chemical composition spectrum,17 characteristic components corresponding to the four drugs were preliminarily inferred from rat plasma samples after administration,including 4 anthraquinones,8 flavonoids,3 alkaloids and 2 terpenes.2.Qualitative identification of Siji Sanhuang pillsOn the basis of the current standard of Siji Sanhuang pill,the microscopic identification items were added.The microscopic identification tests were carried out on Rhei Radix Et Rhizoma,Scutellaria Radix,Phellodendri Chinensis Cortex and Gardenia Fructus.The microscopic characteristics of each drug in the preparation were obtained,and the microscopic characteristics of Siji Sanhuang pill were preliminarily determined.The TLC identification of four drugs in the preparation was added.Firstly,the preparation method of the test solution was optimized and systematically investigated to determine the preliminary development conditions;Then the systematic methodology validation was carried out,including the sample size,sample method and thin layer plate from different manufacturers.The results showed that the established method could be used for the qualitative identification of Siji Sanhuang pills.At the same time,ICP-MS was used to detect lead,cadmium,arsenic,mercury and copper in Siji Sanhuang pills.The average contents of heavy metals in all batches were far lower than the corresponding standards.3.Study on fingerprint of Siji Sanhuang pillsIn order to comprehensively evaluate the quality of Siji Sanhuang pills and show its overall characteristics,HPLC was used to establish the fingerprint determination method of Siji Sanhuang pills.21 common chromatographic peaks were determined.Through 14 batches of samples,the control fingerprint was generated,and the similarity of all batches was above 0.90.The results showed that the method had good precision,repeatability and stability,and could be used for the quality control of Siji Sanhuang pills.4.simultaneous determination of various index components in sisisanhuang pillsSiji Sanhuang pill contains Rhei Radix Et Rhizoma,Scutellaria Radix,Phellodendri Chinensis Cortex and Gardenia Fructus.At present,the related research reports mainly focus on the determination of anthraquinones in rhubarb,and there are also anthraquinones glycosides in Rhei Radix Et Rhizoma,which play a key role in its purgative function;Scutellaria Radix,Phellodendri Chinensis Cortex and Gardenia Fructus also play an important role in the preparation of anti-bacterial and anti-inflammatory,diarrhea and antipyretic.In this chapter,on the basis of experimental exploration and literature research,the content determination of total anthraquinones,free anthraquinones and two anthraquinones glycosides(sennoside A and B)in Siji Sanhuang pills was studied.An HPLC method was established for the simultaneous determination of seven main components in Siji Sanhuang pills except rhubarb,which made the content control of Siji Sanhuang pills more comprehensive.