The Uniformity Of The Production Process Of Angong Niuhuang Pill And The Identification Of Niuhuang Medicinal Materials

Angong Niuhuang Wan is composed of Calculus bovis,musk,rhizoma coptidis,radix Scutellariae,radix curcumae and fructus gardeniae,buffalo horn concentrated powder,pearl,cinnabar,realgar and borneol.The productive process of Angong Niuhuang Wan includes crushing,mixing,than add honey into the mixer,pelleting etc.In the blending process,the particle size,density of powder and blending time have a great influence on the blend uniformity.Therefore,it is difficult to control the quality of mixed intermediates.In addition,there is no way to evaluate the blend uniformity of Angong Niuhuang Wan.Consequently,it is necessary to establish a method to control the quality of blending process.Calculus bovis is a valuable Chinese medicinal herb.Nowadays,due to the limited source and high market price,the substitutes,artificial and in-vitro cultured Calculus bovis,are getting more and more commonly used.The adulteration phenomenon is serious.Therefore,it is crucial to establish a fast and simple method in discriminating the natural,artificial and in-vitro cultured Calculus bovis.In this paper,a novel approach named VO-MBSD was used to characterize the blend uniformity of original powder using Near Infrared Spectrum(NIR)technology,and validity of this method was confirmed by HPLC.Under the condition of pilot production,a method of in-line evaluation of blending uniformity using NIR technology was found,which was used to control the qulity of actual blending process production.Furthermore,a method of evaluation of blending uniformity using Near Infrared Spectrum chemical image(NIR-Cl)was established.In addition,A rapid and straightforward analytical tool for the identification of bezoar and artificial bezoar powder using Near Infrared microspectroscopy is presented,and a new method for identification natural,artificial and in-vitro cultured Calculus bovis was established by using HPLC-MS.First,The study of the influence of particle size and blending time on the unifonnityIn this work,a novel approach named vector operation moving block of the standard deviation(VO-MBSD)was used to characterize the original powder blend uniformity using NIR technology,including Rhizoma Coptidis,Radix Scutellariae,Radix Curcumae and Fructu,s Gardeniae of three different patical sizes,whose mesh were 80,100 and 120.In conclusion,Particle size has a great influence on the mixing uniformity,the mixing time of powder of 100 mesh was shortest.This method can be used for the determination of Chinese traditional medicine powder blending uniformity.Second,The research of real time monitoring of blending process using NIRUnder the condition of pilot production,in line quantification of powder by NIR was found,and validity of this method was confirmed by HPLC.The results of two methods were coincident.The end-point of blending is a period changes between 35min～50min.In conclusion,this method is a good way to control the quality of the blending process of Angong Niuhuang Wan,which provides the theoretical and practical guidance for the determination of mixing uniformity.Third,Research on spatial distribution and composition uniformity of Angong Niuhuang Wan intermediateNIR-CI served as a process analysis technology in the evaluation of Angong Niuhuang Wan blending uniformity.The spatial component distribution was visualized using BACRA method.Then change the intermediate of correlation imaging figure into Lab model figure,and use the K-mean clustering allgorithm to extract the distribution area of buffalo horn.At last,by calculating the distribution area of buffalo horn in each of the pixels,establish a mixed uniformity image evaluation method was established.The spectral imaging technique could be used to construct the spatial composition distribution and composition uniformity of the Traditional Chinese Medicine,Fourth,the identification of bezoar and artificial bezoar powder using Near Infrared microspectroscopyA rapid and straightforward analytical tool for the identification of Calculus bovis and artificial Calculus bovis powder using Near Infrared microspectroscopy is presented.Two qualitative methods were selected to establish identification model.The Principal Component Analysis was used to observe the spatial distribution of bezoar and artificial bezoar.The Discriminant Analysis was used to determine the classes of bezoar and artificial bezoar by computing their distance from each class center in Mahalanobis distance units.Different data pre-processing methods were explored before modeling with the discrimination rate as indicator.The results showed that there is a great difference in principal component spatial distribution.The predictions obtained were quite accurate.In conclusion,Near infrared microspectroscopy could act as an effective method of distinguishing Calculus bovisfrom artificial Calculus bovis.Fifth,A New Method for Identification of Natural,Artificial and in-Vitro Cultured Calculus bovis using HPLC-MSNatural,artificial and in-vitro cultured Calculus bovis were differentiated by bile acids analysis.A new compound with protonated molecule at nz/z 405 was found,which we called 3a,12a-dihydroxy-7-oxo-5β-cholanic acid.This compound was discovered in in-vitro cultured Calculus bovis,but almost not detected in natural and artificial Calculus bovis.A total of 13 constituents were identified.Among them,three bio-markers,including glycocholic acid(GCA),glycodeoxycholic acid(GDCA)and taurocholic acid(TCA)were detected in both natural and artificial Calculus bovis,but the density of TCA was different in two kinds of Calculus bovis.In addition,the characteristics of bile acids were illustrated.In Conclusions,The HPLC coupled with tandem mass spectrometry(LC/MS/MS)method was feasible,easy,rapid and accurate in identifying natural,artificial and in-vitro cultured Calculus bovis.