The Systematic Identification Of Borax Based On XRD,NIRS And Raman Spectroscopy And The Study On The Stability Of Cobalt Irradiation From 4 Kinds Of Traditional Chinese Medicine Such As Borax

Objective Borax,as one of the commonly used mineral Chinese medicine,has a long application history.Borax is a white mineral with many adulterant species;Borax minerals from natural sources and processed products with medicinal materials may contain impurities;at the same time,Borax has not yet Chinese medicinal materials standard.Therefore,the quality evaluation of Borax is an important part to ensure the safety of drug use.This research attempts to systematically study Borax from its historical evolution,quality evaluation standards and modern identification methods,in order to provide a new standard and analytical method for the quality control of Borax.Method 1.Herbal authentication and quality evaluation First of all,this paper is to examine ancient medical books and focuses on the base resource of Borax,origin change,quality evaluation and collection processing,at the same time,through the modern domestic and foreign literature research,the functional treatment and clinical application of Borax were analyzed.In addition,the paper collates the contents of the evaluation of Borax quality in the calendar edition of China Pharmacopoeia and local standards,and summarizes the methods and quality evaluation indexes suitable for Borax quality control.2.Establish standards for medicinal materials and specifications At present,the great majority of Borax medicinal materials in our country are refined with Borax raw materials or industrial Borax,it is necessary to carry out quality evaluation to distinguish specifications.A large number of samples of Borax were collected from various markets,and the quality status of Borax medicinal materials was summarized;the identification,analysis and collation of different medicinal materials from different sources were carried out by the classic methods of character identification and physicochemical analysis.3.Establishment of XRD,Raman and NIRS Analysis Method for Borax On the basis of the above research,and on the basis of XRD method to determine the base source,the Raman spectrum and near infrared spectrum analysis of Borax,and combined with correlation coefficient method,clustering analysis,PLSR and other chemical metrology algorithms,the rapid qualitative and quantitative model of Borax mineral medicine,the rapid system identification and quality evaluation of Borax.3.1 XRD analysis of Borax The XRD spectra of 13 batches of Borax samples were collected,and the peak finding and phase retrieval were carried out by JADE 6.0.The XRD spectra of Borax samples was compared with PDF12-0258(Borax)of standard card and compared with powder XRD map of alum and white Halite with easy mixture.3.2 Raman analysis of Borax On the basis of XRD analysis,the Raman spectral characteristics of each sample were analyzed.Raman fingerprint was established based on the average of 8 batches of Borax positive products and the 10 common peaks of the median.Taking the correlation coefficient of the sample as the similarity evaluation index,the similarity evaluation and clustering analysis were carried out to establish the Raman spectral qualitative analysis method for Borax samples.A Raman spectrometric quantitative analysis model of sodium tetraborate in Borax was established by partial least squares regression(PLSR)algorithm.60 batches of Borax samples were collected,Raman spectra were collected and 60 batches were divided into training and test sets.The content of sodium tetraborate was determined by acid-base titration and used as reference value.Then,abnormal sample culling,spectral pretreatment method screening,model spectrum screening,the training set spectral data and content reference data determined after the screening match with PLSR algorithm,calculate the correlation,and construct PLSR quantitative analysis model.The model is optimized by cross verification in the training set,and cross verification in the internal set is verified by one method.After model optimization,the model prediction ability is investigated by test set.3.3 NIRS analysis of Borax The fast qualitative and quantitative analysis model of Borax was established by using near infrared spectroscopy,which also provided a new rapid analysis method for the quality control of Borax.Under the condition of different spectral pretreatment,the mean spectra of Borax samples were used as reference spectra,and the correlation coefficients between all samples and non-reference spectra were calculated in the whole spectral range.A qualitative analysis model of Borax was established.At the same time,the near infrared spectrographic PLSR quantitative analysis model of sodium tetraborate in Borax was established by using the Raman spectrometric quantitative modeling method.4.The changes of composition before and after irradiation of 4 kinds of Chinese medicine such as Borax were investigated by various techniques Borax,calamine,Halite and Pearl 4 kinds of mineral traditional Chinese medicine powder are often used directly for eye ointment and other external agents.Therefore,sterilization is a key process.In this paper,XRD,near infrared spectroscopy and Raman spectroscopy are used to investigate whether there are significant changes in the fingerprints of these four kinds of medicinal materials before and after 60 Co irradiation,so as to understand whether 60 Co irradiation has any effect on the safety,effectiveness,and quality stability of the products.Result 1.Base and identification of Borax Borax from the " Compendium of Materia Medica ",refers to the same Borax recorded in the modern literature,crystallization of boric acid and Borax,mainly contains sodium tetraborate(Na2B4O7·10H2O).Borax to colorless transparent or white translucent,pure,light and crisp is the best.Both Borax from natural sources and Borax processed from medicinal materials need to be refined,Na2B4O7·10H2O content should be 99%~103%.For the determination of Borax,because of the simple operation of American Pharmacopoeia method,the color change of the end point of titration is obvious,and the titration liquid is convenient and stable.The method is chosen to determine Borax content and the result is calculated by sodium tetraborate.Na2B4O7 shall contain 52.28%~54.39 %,or Na2B4O7·10H2O shall be 99 %~103 %.2.Specification and level of Borax Based on the investigation of a large number of market samples,Borax medicinal materials were found to be classified into Borax block,Borax pendant and Borax powder according to processing method,which are called gradeless and uniformly priced goods in the market.Borax pendant is an irregular bar or conical mass formed by crystallization,with a cotton rope through the center.The properties of Borax,as described in almost all ancient and existing literature,China Pharmacopoeia II and local standards,as well as the 8 samples of Borax that we used X-Ray to confirm are "colorless,transparent,white,translucent" particles,crystals or lumps.Therefore,we intend to meet the content of the required,but the color of a variety of yellow,yellow,brown or gray samples,its grade is defined as "second class",if the internal service,it needs to be further refined.3.XRD,Raman and NIRS Analysis of Borax 3.1 XRD analysis of Borax The XRD pattern of 13 batches of Borax samples was searched for peak and phase.The phase of sample S1-S8 was Borax,S9,S12 and S13 were alum,and S10 and S11 were white sand.The XRD profile of the 8 batches of Borax samples was compared with the standard card PDF12-0258(Borax)and the main components were Na2B4O7·10H2O,so the 8 batches of Borax samples could be accurately identified as genuine.Samples S6 and S8 were white opaque powder which was easily confused with white sand powder;S1,S2,S7 is semitransparent block,similar to the character of Alumen.Compared with Borax,Sal ammoniac and Alumen,there are significant differences in XRD map of Borax.There is also a big difference between Alumen and Sal ammoniac.Therefore,XRD method can be used to identify Borax samples accurately and reliably,and it can provide reliable reference for other analytical methods.3.2Qualitative and quantitative analysis of Raman spectra of Borax A qualitative analysis model of Raman similarity of Borax samples was established.The similarity of Borax products was more than 95% and that of fake products was less than 32%.The result of clustering analysis can also distinguish Borax accurately.After quantitative modeling by Raman spectroscopy,the pretreatment spectra of Borax with maximum-minimum normalization were obtained in the contents of sodium tetraborate between 49.81% and 63.81%.To extract the 1100~700 cm-1 spectrum as the characteristic spectrum,to choose four main causes,A quantitative model of Raman spectroscopy PLSR with sodium tetraborate in Borax was established.The modeling effect and prediction ability of the model are optimal.The maximum deviation of the prediction set is 2.21%,the average deviation is 0.42% and the average relative deviation is 1.62%.The model can meet the requirement of accuracy and precision of traditional Chinese medicine analysis,and the model-to-test set RPD value >3,so it can be applied to the actual analysis.3.3 NIRS analysis of Borax The average spectra of Borax samples were used as reference spectra by using the first derivative as the pretreatment method.When r≥75.45% is authentic Borax and when r<75.45% is counterfeit,the accuracy of the model is 100%.In the quantitative analysis of Borax near infrared spectroscopy,vector normalization and first derivative as a pretreatment method,in 9100~5700 cm-1 spectrum,the quantitative analysis model of Borax was established by interval partial least square method.In internal cross-checking,when RMSECV was 0.36% and R2 was 99.0%,it shows that modeling is effective.In test set validation,when RMSEP was 0.37% and R2 was 98.99%,the maximum relative deviation of the prediction result was 1.02%,the average relative deviation was 0.57% and the average recovery rate was 99.74%,which indicated that the model had good predictive power.4.Stability of the composition of 4 kinds of medicinal materials such as borax before and after irradiation Using the above three analytical techniques has been proved.At the 60 Co irradiation dose of 30 k Gy,the composition of 4 kinds of raw powder including Borax was stable and had no obvious change.Among them,Borax,Calamine,Halite and other mineral drugs and Pearls with mainly inorganic components were analyzed by XRD,which proved that there was no change in the phase and structure of the material.Four kinds of traditional Chinese medicines were analyzed by near infrared spectroscopy,and Borax and Pearl were analyzed by Raman spectroscopy,which showed that the composition and spectrum of Borax and Pearl were stable and had no obvious change.The contents of the main detected ingredients after irradiation are all within the scope of the Pharmacopoeia.Therefore,this study suggests that irradiation can be used to sterilize the 4 kinds of medicinal material powder,but the dose should be appropriate and should not exceed 30 k Gy.Conclusion Through this research,it is proved that Borax is the same source in ancient and modern times.It is the crystal of Borax refined by Borax of Borax salt family of Borax,which contains sodium tetraborate(Na2B4O7·10H2O).Colourless transparent or white translucent,pure,light and crisp Borax is the best.The content of Na2B4O7·10H2O should be 99~103%,which can guarantee the refining degree of Borax,and avoid losing too much water and overdose.On this basis,the standard of Borax Chinese medicine and commodity specification level standards,can guarantee the safety of medication.On the basis of XRD method to determine Borax accurate base,the qualitative and quantitative analysis model of Raman spectrum and NIRS spectrum of Borax is established.In this research,the study of Borax from the basis of traditional Chinese medicine,using XRD,NIRS and Raman modern technology to identify Borax has demonstrative application,and has guiding significance for other mineral drugs.In this paper,a variety of techniques were used to study the changes of composition before and after irradiation of 4 kinds of traditional Chinese medicine powder such as borax.The effects of radiation exposure on the mineral constituents of traditional Chinese medicine were investigated from several angles such as XRD,NIRS and Raman spectra.In order to understand whether 60 Co irradiation has any effect on product safety,effectiveness and quality stability.It provides a reliable basis for the enterprise’s product upgrade and safety evaluation.The above research has enriched the research content of the basic theory of traditional Chinese medicine,and has certain reference significance to ensure the safety and efficiency of the medicine of Borax.