| Objective:Honey pills,a traditional Chinese medicine(TCM)formulation,is widely used in clinical applications.Although the process of refining honey is an important factor affecting the quality of honey pills,it has not been standardized so far,resulting in considerable differences in quality across batches.In this study,LiuWei Dihuang Pill was used as a model drug,and modern analytical techniques and mathematical model fitting methods were used to quantitatively study all aspects of the honey pill molding process,and to establish corresponding mathematical prediction models.In order to provide an experimental basis for the quantitative characterization of the production process of the pill and the prediction of the physical parameters of the Material-pellet,pellet-pill,it can promote the preparation of the pill,optimize the ratio of raw and auxiliary materials and improve the quality of the pill.Methods:this experiment uses modern physical instruments(rotary rheometer,texture analyzer,color difference meter,laser particle size analyzer,etc.)to realize the quantitative characterization of physical property parameters of traditional Chinese medicine powder,refined honey,intermediate pellets and honey pills.Modern data analysis methods such as multiple multiple regression,establishing correlations between drug powder properties,honey-smelting properties,pellet physical properties,and physical properties of final product pills,details as follows:(1)Quantitative characterization of physical properties of raw materials:88 batches of honeys were refined according to the traditional process,and the rheological properties were determined by rheometer.The Liuwei Dihuang Pill was used as a model drug.The smashing method was used to pulverize according to the prescription ratio.Separate densitometers,laser particle size analyzers,and angle of repose indicators were used to determine the powder properties and water content of the powder,in preparation for the later development of the parameters of the physical properties of the powder.(2)Characterization of physical properties of pellets and pills:The physical properties of pellets and pills were characterized by a texture analyzer compression test method.Through the analysis of the texture curve,the literature review,and the feasibility of the test conditions,the physical properties of the pellet hardness,adhesion,elasticity,recovery,compression work,positive work,and adhesion work were selected.Hardness,adhesion,elasticity,recovery,compression work,positive work 6 parameters were used to characterize the physical properties of the pills.(3)Characterization of physical properties of pellets and establishment of mathematical model of "pellet-pill" physical properties:For the quantitative physical parameters of powder,sweetener,pellet and pill in the process of honey pellet forming and multiple regression analysis,the prediction model is established.And the variance R2,predict the residual squared sum and the PRESS model to judge the predictability of the model.After the model is established,the parameters of the powder and the refined honey are determined,and the physical parameters of the pellet and the pellet are predicted by the model;then the preparation and measurement of the pellet are performed,and the difference between the predicted value and the measured value is compared to verify whether the model is successful.(4)Rapid determination of viscosity of refined honey:We developed a near-infrared spectroscopy(NIRS)-based approach to monitor the quality of 88 batches of refinedhoney in real-time,combining the respective viscosities using a rotary rheometer,and obtaining the NIRS spectra,an optimal quantitative model was established throughoptimization of pre-treatment methods,wave bands and principal components.Results:(1)Quantitative characterization and quantitative model establishment of honey-refining properties:The honey viscosity quantitative model was established by the near-infrared spectroscopy method using the viscosity measured by rheometer as the index,which realized the transformation of the refined honey characteristics from fuzzy qualitative description to quantitative.In the quantitative model,the corrected root mean square error RMSEE is 0.084,the correlation coefficient R2 is 99.79,the internal cross-validation RMSECV is 0.089,and the coefficient of determination R2 is 99.74.The RMSEP of the viscosity is 0.085 and the R2 is 99.55.The results show that there is a good correlation between the predicted value and the actual value of the sample,the error is small,and the viscosity of the refined honey can be predicted to a certain extent.The boundary between different refining honey is obvious,and there is obvious clustering phenomenon,which indicates that the factorization method is an effective method to identify honey.Thereby initially determining the scope of the refined honey;Tender honey:200-400mpas,medium honey:500?1900mpas,old honey:2000?6000mpas.(2)Quantitative description experiment of physical properties of powder:the experiment shows that the particle size,angle of repose,bulk density and bulk density of the three fine powders show that the smaller the particle size of the fine powder,the more concentrated the particle size distribution range and the more uniform distribution.The angle of repose is negatively correlated with the particle size of the powder,and the tap density is positively correlated with the bulk density and particle size.Through the quantitative description of the powder powder's physical properties,instead of the subjectively strong empirical judgment,it prepares for the later study of the characteristics of the powder and the honey pellet forming.(3)Characterization of the physical properties of the pellets and the establishment of the mathematical model of the physical properties of the raw materials and pellets:Firstly,the determination parameters of the texture analyzer are optimized,and the optimal conditions are determined according to the magnitude of the coefficient of variation.Then Plackett-Burman experiment was used to screen the significant factors affecting the process of combining the honey pill.The significant factors are selected as independent variables,and the texture properties such as hardness,adhesion and elasticity of the pellet are the dependent variables.All the above factors were mixed by using the full factorial design experiment to prepare different pellets,and then the texture properties such as hardness,adhesion and elasticity of the pellets were measured.Using the method of multiple multiple regression analysis to establish the mathematical model of the physical properties of "Materials-pellets" The model was improved by principal component regression and partial least squares regression.In predicting the physical properties of the pellets,the PRESS of the pellet hardness,adhesion,elasticity,recovery,compression work,positive work,and adhesion work are 20.00,20.33,26.25,13.71,12.34,20.49,14.78,respectively.The predicted variance R2 is 0.7897,0.7833,0.9651,0.7869,0.7774,0.7782 and 0.9166,respectively.The results show that the model is stable.(4)Characterization of physical properties of pellets and establishment of mathematical model of "pellet-pill" physical properties:the factors of various factors were mixed by using the full factorial design experiment,the pellets were prepared according to the plastic method,and then the hardness of the pellets,the texture properties such as adhesion and elasticity were measured.The mathematical model of"pellet-pill" physical property was established by multiple multiple regression analysis.In the model of predicting the physical properties of the pellets,the PRESS of the pellet hardness,adhesion,elasticity,recovery,compression work,and forward work were 15.31,14.72,22.83,23.72,36.40,27.87,respectively,and the predicted variance R2 was 0.8480,0.7423,0.7332,0.7076,0.8485 and 0.6877.From the prediction variance R2 and the prediction residual squared sum PRESS,the prediction model is ideal.That is,multiple linear regression analysis is suitable for predicting the physical properties of pellets and pellets during the production of honey pellets.Conclusion:This topic uses Liuwei Dihuang Pill as a model drug to quantitatively characterize the physical properties of raw materials,intermediates and finished products in the production process of honey pill.The standard of refining honey was established by viscosity,and the viscosity model of different grades of honey was established by near-infrared spectroscopy to achieve rapid determination of the viscosity of refined honey.Objectively describe the characteristics of the powder using a laser particle size analyzer.The texture analyzer is used to characterize the physical properties of the intermediate pellets and the finished pills.The mathematical model of the relationship between material-pill,pellet-pill property parameters in the preparation of honey pill was established by multiple linear regression method and successfully verified.Through this research,it can provide experimental basis for the scientific quantitative transformation of the honey pill process;it is beneficial to establish a quality control system for the preparation of honey pill preparation from fuzzy to precise control;the creation of predictive model guides the production of honey pill;optimizes the ratio of raw materials;and to improve the quality of honey pill molding has important practical significance. |
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