Study On Quality Standard Of Feire Cinnabar Wuwei Pills

Objective: In this experiment,the quality standard of Feire Cinnabar Wuwei Pills was studied as the core,and the quality standard of Feire Cinnabar Wuwei pills was preliminarily improved through character identification,physical and chemical identification,thin layer identification,content determination and various examination methods.Method: According to the Chinese Pharmacopoeia(2015 edition)and the methods,the characters of Hanshishui Shi,Tianzha huang,licorice,cinnabar,fritillaria chuanensis and other medicinal materials in this preparation were identified,the microscopic identification of licorice,fritillaria chuanensis and cinnabar,the physical and chemical identification of cinnabar and Hanshishui Shi,and the TLC identification of licorice and fritillaria chuanensis were conducted.The content of glycyrrhizin and ammonium glycyrrhizinate in the preparation were determined by HPLC and the amount of mercury sulfide in the preparation was determined by coordination titration method.And according to the Chinese Pharmacopoeia(2015 edition)related methods to check the preparation of moisture,ash,extract and pack volume difference,weight difference,dispersion time,etc.The TLC identification of Glycyrrhizae was performed by TLC(General Code 0502).Three batches of preparation test solution,1~2μl of control medicine solution and negative control solution were collected,and ethyl acetate: formic acid: glacial acetic acid: Water(15:1:2)was used as the developing agent,developed,took out,dried,sprayed with 10% sulfuric acid ethanol solution,heated at 105℃ until the color was clear,and inspected under ultraviolet light(365nm).In the chromatogram of the test product,fluorescent spots with the same color were displayed at the corresponding position of the chromatogram of the control medicinal materials.The TLC identification of fritilin B was performed according to TLC(General Rule 0502).Three batches of preparation were collected,5~10μl of test solution,reference solution,reference medicinal material solution and negative control solution,and ethyl acetate: petroleum ether:methanol: Ammonia water(10:10:2:1)for the development of the agent,expand,take out,dry,iodine powder several times embedded to the color clear,test product chromatography,in the position corresponding to the control medicine chromatography,show the same color spots;Show spots of the same color on the position corresponding to the chromatogram of the reference.The content of glycyrrhizin and ammonium glycyrrhizinate in this preparation was determined by HPLC.The chromatographic conditions were as follows: Using octadecylsilane bonded silica gel as the filling agent,acetonitrile as mobile phase A and 0.05% phosphoric acid as mobile phase B,the gradient elution was carried out according to the relevant regulations of licorice decoction pieces in Chinese Pharmacopia(2015 edition).The detection wavelength was set at 237 nm,and the column temperature was 30 ℃.The content of mercury sulphide in this preparation was determined by coordination titration and titrated with ammonium thiocyanate(0.1mol/L).Each 1 m L of ammonium thiocyanate titrator(0.1mol /L)corresponds to11.63 mg of mercury sulfide(HgS).Results: The medicinal materials in the preparation all met the identification standards of Chinese pharmacopoeia(2015 edition).Microscopic identification results: irregular fine particles dark red,shiny,dark black margin(cinnabar).The parenchyma cells surrounding the fibrous bundles contain calcium oxalate square crystals that form crystalline fibers(licorice).Starch granulae are faintly seen(Fritillaria chuanensis).When using TLC to identify licorice and fririformin B in Feirezhusha Wuwei Pill,spots of the same color(fluorescent spots)were shown in the chromatographic position corresponding to the control material and the control material,and no spots of the same color were shown in the corresponding position of the negative control.The results of content determination showed that the linear equations of glycyrrhizin and ammonium glycyrrhizinate in this preparation were Y = 1.0138X+0.0065,Y = 0.0826X+0.0308,and the correlation coefficient was: R =1,R =0.9999,indicating that the peak area of glycyrrhizin and ammonium glycyrrhizinate was linear in the range of0.9983~19.9925(μg/m L)and 9.814 ~199.4983(μg/m L),respectively.The contents of glycyrrhizin and glycyrrhizic acid in three batches of samples were 1.4444-1.5223 μg/m L and 21.8134~23.2869 μg/m L,respectively.The average contents were 1.4869μg/m L and 22.4524μg/m L,respectively.The water content of this preparation was 3.66% ~ 5.07%.Ash content: 4.81% ~6.0%;Water-soluble extract: 8.69% ~ 20.8%(hot immersion),4.77% ~ 6.31%(cold immersion),alcohol-soluble extract: 3.8% ~ 18.6%(hot immersion),3.40% ~ 6.10%(cold immersion).Weight difference,packing volume difference and dissolving time limit are all in accordance with the relevant regulations of Chinese Pharmacopoeia(2015 edition).Conclusion: The experimental results show that the identification and content determination method used in this paper is advanced,simple,specific,repeatable and accurate,which provides an effective basis for improving the quality standard of Feire Cinnabar Wuwei pills.