Study On The Preparation And Quality Standard Of The Sixteen Flavors Azalea Concentrated Pill

Objective:To study the prescription of the Sixteen Flavours Azalea Concentrated Pill and the establishment of draft quality standards.Methods:（1）Nine herbs In Prescription,namely Semen punicae granati,Carthami Flos,Calcaria,Radix et Rhizoma Rhodiolae kirilowii seu bergeniae,Glycyrrhizae radix et rhizome,Choerospondiatis fructus,Bibo piperislongifructus,Raisin,Eriocheiris seu potami were extracted by heating and refluxing.Using L₉（3⁴）orthogonal test method,taking the comprehensive score of Hydroxysaffron Yellow A,Total Flavonoids and dry extract as the index,taking the extraction times,extraction time and water addition multiple as three levels,the extraction process of the intermediate of Sixteen Flavours Azalea Concentrated Pill was studied,and the method for determining the content of Hydroxysaffron Yellow A and Total Flavonoids in the intermediate was established.（2）Taking the appearance,size and dissolution time of the pills as the investigation indicators,the single-factor investigation method was used to determine the prescription and preparation process of Sixteen Flavors Azalea Concentrated Pill.Three batches of amplification experiments were carried out to verify the rationality of the prescription and the stability of the preparation process;（3）Different irradiation doses were used to irradiate the Sixteen Flavors Azalea Pill by electron accelerator,and the changes in the properties,microscopic characteristics,thin layer chromatograms of sedum herb and active ingredient piperine,the content of active ingredient Hydroxysaffron Yellow A and the similarity of high performance liquid chromatograms,as well as the total bacterial colony count and total mould yeast colony count of the Sixteen Flavors Azalea Pill were compared before and after irradiation,respectively.and the effects of electron beam irradiation on the main active ingredients and sterilization effects of Sixteen Flavor Azalea Pills,and the applicability of electron beam irradiation sterilization;（4）Taking the amplified experimental sample as the research object,with reference to the quality regulations of the 2020 edition of the Chinese Pharmacopoeia,establish a thin-layer chromatographic identification method for Cinnamomi Cortex,Aquilariae Lignum Resinatum,Radix Et Rhodiolae Kirilowii Seu Bergeniae,Choerospondiatis Fructus in concentrated pills,a method for determining the content of Hydroxysaffron Yellow A,Benzyl Acetone and Total Flavonoids,and formulate quality standards（draft）for concentrated pill.Results:（1）The results of the intermediate extraction process show that the optimal extraction process of the intermediate of Sixteen Flavor Azalea Concentrated Pill is 10times the amount of water,extracted 3 times,1 h each time,and the experimental results of 3 batches verify that the repeatability of the extraction process is good;（2）The forming process for the Sixteen Flavors Azalea Concentrated Pill is to powder the seven herbs,namely Flos Rhododendrianthopgonoidi,Aquilariae Lignum Resinatum,Aucklandiae Radix,Cinnamomi Cortex,Amomi Fructus Rotundus,Myristicae Semen,Caryophylli flos to a fineness of 100 mesh;the rest of the herbs are extracted and filtered according to the best extraction process,and the filtrate is concentrated to a thick paste with a density of 1.06 at 80°C under reduced pressure;the thick paste,powder and Sodium Carboxymethyl Cellulose binder are mixed,then 10%ethanol is added,and The ratio of raw material:auxiliary material:wetting agent was fixed at52:2:5,mixed well,and the pills were prepared by the plastic method and dried in an oven（30°C）for 6 h.（3）After sterilization by different doses of electron accelerator irradiation,there was no significant effect on the properties,the powder microscopic characteristics、the thin-layer chromatogram of Aquilariae lignum resinatum and active ingredient piperine of Sixteen flavor azalea pill.There was no significant difference in the content of Hydroxysaffron Yellow A（P>0.05）and chromatogram similarity analysis is 1.000.The number of bacteria and the total number of molds and yeasts were significantly reduced after irradiation with different doses of electron accelerator（P<0.05）.When the electron accelerator irradiation dose is 8 k Gy and above,the microbial limit of the sample conforms to the 2020 edition of the Chinese Pharmacopoeia.（4）The four flavor medicinal materials of Cinnamomi Cortex,Aquilariae Lignum Resinatum,Radix Et Rhodiolae Kirilowii Seu Bergeniae,Choerospondiatis Fructus in concentrated pill were qualitatively identified by TLC,and the spots were clearly colored and negative without interference.The content of Hydroxysaffron Yellow A/Total Flavonoid/Benzyl Acetone in concentrated pill was determined by HPLC/UV/GC method,the established method was simple and easy,high accuracy and strong operability,the content of Hydroxysaffron Yellow A in three batches of amplified experimental samples was 0.435 mg/g,the content of Benzyl Acetone was 0.076 mg/g,and the Total Flavonoids was 2.431 mg/g,and all inspections of the three batches of samples complied with the provisions of the Chinese Pharmacopoeia on pill.The established quality standard（draft）can effectively control the quality of the sample.Conclusion:The intermediate extraction process of Sixteen Flavor Azalea Concentrated Pill optimized in this experimental study has good repeatability,the prescription of concentrated pill is scientific and reasonable,the preparation process is stable and reliable,the irradiation sterilization process confirms that it can effectively reduce the level of microorganisms,and has no significant impact on the main index components,and the quality control method is simple,accurate,stable and operable,which can be used for the quality control of the preparation.