Study On The Processing Mechanism Of Realgar Shuifei And The Quality Of Its Decoction Pieces

Red arsenic comes from the mineral sulfide realgar family,It was first recorded in the han "Shen Nong Ben Cao Jing",powder-refining methord with water was first seen in the song "key to children's diseases".The character of it is pungent,warm.It has been used to detoxification,drying dampness and resolving phlegm,pesticides in clinical.There are not special regulation when it comes to the internal that we use realgar powder.The standard of Arsenic in"China pharmacopoeia"(2015 edition)is the same to the China pharmacopoeia(2010 edition).Pharmacopoeia of realgar processing was water levigating,but the method of it was light on details.Pharmacopoeia said that the arsenic in the realgar with arsenic sulfide(As2S2)shall not be less than 90.0%.Processing of realgar should be the water levigating.While the limit test of it could not contain the amount of arsenic.Parts of local Chinese medicine preparation also contain dry grind realgar.The topic is a part of security and control in ten kinds of topical preparations which medicinal minerals was contained.The reachers make extension to some extent.At present,how to investigat the amount of commercial arsenic,whether it was processed by water or not.It still needed to inspection.The study aims to investigate that with particle size uniformity,water levigating realgar compared with dry grind realgar its influence of the ingredient type and toxicity,to elaborate the principle of shuifei processing.We also examined the quality of the realgar which were sold in the market.Objective:Particle size,color and quantity of arsenic were studied in different processed products of realgar;Water levigating reaglar:morphology elemental analysis,content of solubility arsenic and total arsenic combined with acute toxicity experiment were considered to expound the processing principle of levigation initially.titration of pharmacopoeia and X-ray diffraction technology were used to examine the quality and to guarantee the validity and authenticity of the sold realgar.To determine the quality of reaglar in the market,particle size,color and quantity of arsenic were investigated.Methods:The study were prepared realgar with water levigating product,grinding product which hasten to water levigation,grinding product,water washing product,30%acetic acid levigating product,30%acetic acid washing product,0.2%hydrochloric acid levigating product,0.2%hydrochloric acid washing product.11 samples which come from different places were collected,two of them 8 processed products are prepared,while the rest of the samples only prepared the water levigation and grinding product which hasten to water levigation.1 The laser particle size distribution was used to measure the size of various products with deionized water as dispersion medium and the experimental results was analysed by SPSS20.0 cluster software.2 Chromatic measuring was used to determine the color of the processed products,the experimental results was analysed by SPSS20.0 cluster software and SIMCA-P+12 software.3 Content of arsenic disulfide in different processed arsenics were measured by the method adopted in pharmacopeia.4 With the connection of XRD and High score plus software to determine the phase composition and crystal structure of realgar.5 The scanning electron microscope(SEM)was used to observe the surface morphology of different processed products at 10000 times microscope.SEM-EDS was used to determine elements species and content of each processed products.6 Hydride generator-atomic absorption was used to determine the content of soluble arsenic,which extracted in artificial intestinal juice.7 Realgar samples are digested by microwave,the content of total arsenic are determined by atomic absorption spectrophotometer.8 Toxicity experiment was designed with Mice's intoxication reaction and mortality were observed after administration for 14 days,LD50 and 95%confidence interval were obtained by SPSS20.0 software.9 Content of arsenic disulfide,soluble arsenic,total arsenic in the sold realgar were measured by iodometry and AAS technique respectively.X-ray diffraction(XRD),laser measurement and chromatic measuring were used to determine the phase composition,particle size and color of difference realgar which were sold in the market.Results:1 The particle size of 8 kinds of processed products from the two localities and 2 kinds of processed products from the nine localities were tested.With the sample from Guizhou XH-7 as an example cited the particle size of D50 Water levigating:9.54?m,grinding product which hasten to water levigating:8.41 ?m,grinding:19.03?m,water washing:19.39?m,30%acetic acid levigating:8.18?m,30%acetic acid washing:19.66?m,0.2%hydrochloric acid levigating:9.70?m,0.2%hydrochloric acid washing:19.44?m.The results showed that the D50 mostly at the range of 10?13 microns after levigation,while the D50 at the range of 15?20 microns after grinding and washing treatment.The clustering analysis with SPSS20.0 levigation and hasten to levigation gathered for a class,while washing and grinding samples gathered for a class.2 The color of 8 kinds of processed products from the two localities and 2 kinds of processed products from the nine localities were determined.Founding that after water levigating processing the L*mostly ranged from 59 to 67,a*mostly ranged from 31 to 44,b*mostly ranged from 52 to 70.3 The content of arsenic disulfide of 8 kinds of processed products from the two localities and 2 kinds of processed products from the nine localities were tested.With the sample from Guizhou XH-7 as an example cited the content of arsenic disulfide.Water levigating:94.01%,grinding product which hasten to water levigating:93.13%,grinding:92.77%,water washing:93.43%,30%acetic acid levigating:94.67%,30%acetic acid washing:94.05%,0.2%hydrochloric acid levigating:94.52%,0.2%hydrochloric acid washing:93.61%.The content of arsenic disulfide in different processed products of comparison:levigating>washing>grinding realgar.4 Medicinal realgar mainly contain alpha configuration(AsS)and/or beta configuration(As4S4).The associated minerals are mainly silicon dioxide(SiO2)and orpiment(As2S3),while arsenic trioxide(As2O3)has not been detected.5 When the microscope observation of SEM was 10000 times,the levigating samples had more obtuse and smooth surface with adherent powder.The hasten to water levigation had more than a polygonal.6 Using SEM-EDS to measure the elemental categories and quantities,then analyzed by weight percentage of arsenic and sulfur element finding the gross of them was more than 90%.By comparision the ratio of the atomic percentage of arsenic and sulfur,the levigation was near by 1.1,the sample hasten to water levigation was around 1.3.7 Using Hydride generator atomic absorption to determine the content of soluble arsenic of realgar processed products.The content of soluble arsenic of levigation samples were much higher than the sample hasten to water levigation.the values of the levigation was 1.5%?5.0%.8 The contents of total arsenic in realgar processed products were determined by FAAS,the results of total arsenic in water levigating realgar was significantly higher than grindind ones.9 LD50 obtained from different processed sample was 9.312g/kg,11.852g/kg respectively.10 The contents of arsenic disulfide in sold realgar were tested.All of them were less than 90%.Using XRD to measured the main ingredient of XH-18 finding that silica was the main ingredient of it.The D50 of sold realgar mostly ranged from 3 to 20 microns.The L*a*b*of sold realgar mostly around 50,30,40 respectively.Besides one sample,the content of soluble arsenic of the rest sold samples were less than 1%.The results of total arsenic were almost same or increases slightly,which compared with the determination of iodometry.Conclusions:1 By analyzing the particle size result,finding that D50 of water levigating ranged from 10 to 13 ?m.Washing could not chang the size of it.2 The size of the particle can influence the color of the proceed realgar,the smaller the particle size,the greater yellow and flamboyant the color.3 The contents of arsenic sulfide in various processed products of realgar were greater than 90%,principal component content of water relevigation increased,showed that flying method can remove the impurity.4 XRD analysis results found realgar principal component should be As4S4 or AsS,2015 edition fix that the major ingredient of it should be As2S2.There are some problems in Chinese pharmacopoeia provisions.5 According to the observation of SEM at 10000 times microscope,we can distinguish the water levigating realgar and dry grind realgar.6 According to the aggregate value of arsenic and sulfur element weight percentage could evaluate weather the quality meets the Pharmacopoeia.After water levigating treatment its ratio significantly smaller than grinded ones.It indicated that after shuifei treatment the toxic ingredient of realgar dislodged.7 The source of realgar was an important factor affecting the content of soluble arsenic.When the sizes were uniform,the content of soluble arsenic in water levigating realgar were significantly higher than the grinded ones.The dissolution increased,which means improving the efficacy.8 With the connection of XRD and iodometric shows that processing with realgar can remove impurity;the difference between the ratio of arsenic and sulfur atom reduced,indicating that wate processing can reduce poisonous effect,while the dissolution of soluble arsenic increased.Overall realgar processed with sheifei treatment reached the action of impurity attenuation and synergy,while the synergy is likely to be stronger than the attenuated.9 The powder of realgar sold in the market mostly fake.The arsenic stain method can not to guarantee the quality of it.The quality control index of it is too single.The powder of realgar with wider range.The color of water levigatiions were much bright,colorful,and yellow.than it.We suggest pharmacopoeia to increase the method of particle size and color to control the quality of it.