| As a traditional Chinese medicine,Xinyi was used frequently in our country,which is the dry flower bud of Magnolia biondii,Magnolia denudata,Magnolia sprengeri.It is often used to treat wind-cold,headache and all kinds of rhinitis,face black spot with high medicinal value.According to the 2015 edition of Chinese Pharmacopoeia,the content of volatile oil(?1.0%mg/ml),magnolia(?0.40%)and water(?18.0%)were limited and regarded as the index to evaluate the quality of Xinyi.However,pharmacological effects of the traditional Chinese medicine are rooted in multi-component interaction.It can be seen that it is more accurate to analyze the whole medicine when quality control is carried out.In the quality control study of traditional Chinese medicine,the index components are often determined by conventional techniques such as HPLC,GC,UV and etc..Nevertheless,these traditional quality analysis techniques have some disadvantages including cumbersome operation,time-consuming and laborious,high cost and pollution in the analysis process.As a green analysis technology in recent years,Near-Infrared Spectroscopy has been widely applied in the quality analysis of traditional Chinese medicine due to its advantages of convenience,celerity,highly efficiency,low cost,no harm to samples,no reagent consumption,and no pollution to the environment.In this study,it was systematically discussed how to develop the comprehensive quality control method of Xinyi by combining conventional detection method,Near infrared Spectroscopy and Chemometrics,with a simple,fast,environmental protection,efficient and accurate quality control evaluation system being established.which provided new ideas and methods for the quality evaluation of TCM.At the same time,it is of great practical value to provide strong support for the modernization research of Chinese medicinal materials.Aimed at the above research objectives,the main contents and results of this study are summarized as follows:Firstly,the contents of 13 index compounds in Xinyi were determined.On the basis of consulting a large number of literatures,the systematic analysis method combined pharmaceutical analysis with pharmacochemistry was proposed to prepare volatiles,water-soluble extractive and lignans parts from the same sample.This way could extract more index components to be beneficial in the quality control of Magnolia biondii Pamp.roundly.Then,we developed a Gas chromatography-mass spectrometry separation method for the qualitative and quantitative analysis of volatiles,together with a High-performance liquid chromatography-mass spectrometry separation method for lignans in Magnolia biondii Pamp..79 volatiles and 11 lignans were identified via comparing their chromatographic behavior and mass spectra data with those in the literature.The methods were then used to determine the contents of volatiles(1,8-cineole,D-Limonene,?-terpineol,linalool,L-camphor brain and bornyl acetate)and lignans(epieudesmin,magnolin,epi-magnolin A and fargesin)in Magnolia biondii Pamp..Secondly,NIRS quantitative analysis models for index compounds of Xinyi were established.13 qualitative models were developed by Near-Infrared Spectroscopy based on partial least square regression herein.The values of the coefficient of determination of internal cross validation(R~2)of D-Limonene,1,8-cineole,?-terpineol,linalool,L-camphor brain,bornyl acetate,water-soluble extractive,pinoresinol dimethyl ether,magnolin,epi-magnolin A,fargesin and moisture were0.9713,0.9831,09746,0.9778,0.9731,0.9708,0.9705,0.9822,0.9914,0.9817,0.9920,0.9919,0.9850;the values of root mean square error of calibration were 0.0992,0.4630,0.0071,0.0249,0.0037,0.0580,0.0064,0.0021,0.0808,0.1390,0.0253,0.0211,0.2880;the values of root mean square error of prediction were 0.0838,0.3980,0.0065,0.0213,0.0032,0.0496,0.0055,0.0019,0.0690,0.1200,0.0211,0.0210,0.2810;the values of root mean square error of cross validation were 0.2864,1.4701,0.2052,0.0730,0.0051,0.1170,0.0167,0.0084,0.1535,0.2691,0.0710,0.0408,0.3827,respectively.And the values of the ration of standard deviation of the validation set to standard error of prediction(RPD)to verify the performance of models were no less than 5.The results showed that the NIRS quantitative analysis models are accurate,stable and reliable,and it can be used for the rapid measurement of the content of index compounds in Xinyi.Thirdly,Near-infrared spectroscopy and electronic nose techniques were used to distinguish Xinyi from different producing areas.The results showed that only the NIRS techniques had a good degree of discrimination in different producing areas,and the models could be used for the classification of Xinyi from different producing areas. |
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