| Standards lead the development of the industry.Near infrared(NIR)spectroscopy has been widely used in agriculture,petrochemical,pharmaceutical,food and other fields due to its advantages of convenient operation and fast analysis.However,due to the variety of NIR instruments and the difficulty of analysis and modeling,the development of standard analysis methods is relatively slow.Therefore,in the pharmaceutical field,near-infrared related standards are few and far between.Blending uniformity and water content are the crucial quality attributes in the production of traditional Chinese medicine(TCM),which are of vital importance to the safety and effectiveness of the final product.However,the traditional control method of blending uniformity not only squanders time and vigour,but also interferes with the blending,even destroys the blending balance,resulting in errors easily.Similarly,Similarly,the traditional method of determining water content takes a long time and requires high conditions.Not only the operation is cumbersome and time-consuming,but also the water content often changes in the determination process.Therefore,in order to ensure the stability and uniformity of the final product quality,it is imperative to detect the blending uniformity and water content in the production process of traditional Chinese medicine(TCM)by NIR spectroscopy.However,although many traditional Chinese medicine manufacturers have adopted this technology for the detection of blending uniformity and water content at present,there is no unified standard,and the NIR detection method standards have not been reported so far,leading to related production enterprise technology and quality inspection reports multifarious,which restricts the application,quality control and traceability of NIR spectrum technology.Therefore,based on the process analysis technology,this study took Tongren Niuhuang Qingxin Wan and the extract powder of Yinxingye as carriers,aiming at the standard target,and established the NIR detection methods for blending uniformity and water content respectively.Finally,based on the multi-batch research of multiple dosage forms,combined with the universality,applicability,standardization and authority of the standard,the group standard for the NIR spectral determination of the mixing uniformity and water content of traditional Chinese medicine was established.The main research contents include the following three parts:1、Establishment of near infrared on-line detection method for powder mixing uniformity in the production process of traditional Chinese MedicineIn this chapter,Wuji Baifeng pill,Naoxintong capsule and Jianwei Xiaoshi tablet were used as research carriers.Luminar 4030 online near-infrared spectrometer,GSA101A online near-infrared spectrometer,SNAP321 Software package and the unscrambler chemometrics software were used to determine the mixed end point online.According to the reference method,the method can be used to detect the mixing uniformity of Wuji Baifeng pill,Naoxintong capsule and Jianwei Xiaoshi tablet on-line,and judge the mixing end point accurately.In the actual production process,the method established in this research has good application value for the quality control of the above carriers.2、Establishment of group standard "On-line detection of powder blending uniformity in the production of traditional Chinese medicine Near infrared spectroscopy"Taking Wuji Baifeng Wan,Naoxintong capsule and Jianwei Xiaoshi tablet as carriers,according to the previous work foundation and field investigation of the research group,combined with the mixed online data collected by different mixing equipment and NIR spectrometer provided by the company of Shandong Jinzhang Longxiang,Collected and analyzed 223 expert opinions from working groups,universities,research institutions and related product production units in related industries in China,and gradually formed the preliminary draft,the draft for comments and the draft for review,and finally established a group standard" On-line detection of powder blending uniformity in the production of traditional Chinese medicine Near infrared spectroscopy ",and completed " Standard Appendix "and" Compilation Instructions ".3.Establishment of near infrared detection method for water contentWith the extract powder of Yinxingye,intermediate particles of Yinxingye and Tongren Niuhuang Qingxin Wan as the research carriers,the quantitative analysis model of water content based on partial least square method(PLS)was established by NIR spectroscopy.The first derivative,Savitzky-Golay filter smoothing,multi scatter correction(MSC),standard regular variation(SNV)and other spectral pretreatment methods were compared to optimize the quantitative model of water content with the following model evaluation indicators such as root mean square error(RMSEC),cross validated root mean square error(RMSECV)and determination coefficient(R2).The results showed that in the quantitative analysis of the water content of the extract powder of Ginkgo biloba leaf,the best spectral pretreatment method is SG9+SNV,the number of main components is 4,Rpre2 is 0.9373,and the RMSEP is 0.2471.The bias is 0.03353,and the average relative error is 5.04%.In the quantitative analysis of the water content of the intermediate particles of Ginkgo biloba,the best spectral pretreatment method is Normalize,the number of main components is 5,Rpre2 is 0.9266,and the RMSEP value is 0.3282.The bias is 0.0396,and the average relative error is 4.18%.And in the quantitative analysis of the water content of Tongren Niuhuang Qingxin Wan,Rpre2 and RMSEP with packaging film samples were 0.7657 and 0.1572,respectively,with an average relative error of 1.15%;Rpre2 and RMSEP without packaging film samples were 0.7722 and 0.2078,respectively,with an average relative error of 0.62%,indicating better prediction results.It shows that the water NIR quantitative model has good prediction performance.4、Establishment of group standard " Non-destructive determination of water content of intermediates and preparations in the production Process of traditional Chinese medicine Near frared spectroscopy"Taking the extract powder of Yinxingye,intermediate particles of Yinxingye and Tongren Niuhuang Qingxin Wan as carriers,according to the work foundation of the research group in the early stage,and combined with the research content of the third chapter of this study,the preliminary draft,the draft for comments,standard appendix and the compilation instructions of the group standard " Non-destructive determination of water content of intermediates and preparations in the production Process of traditional Chinese medicine Near frared spectroscopy " have been gradually completed. |
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