A Study On Quality Control Of Lonicerae Japonicae Flos Herbs And Preparations Based On Near Infrared Spectroscopy

Lonicerae Japonicae Flos(LJF,Chinese name is jingyinhua)is the dried flower buds or the first blooming flowers of the Lonicera japonica Thunb.,which has the functions of clearing heat and detoxifying,and dispersing wind heat.Many reports have shown that it has obvious pharmacological effects such as antibacterial,anti-inflammatory,antipyretic,antiviral,and liver protection.It has been used as a raw material for functional beverages,tablets and oral liquids of different brands.Lonicerae Flos(LF,Chinese name is shanyinhua)is the dry bud or the first blooming flower of Lonicera macranthoides Hand.-Mazz.,Lonicera hypoglauca Miq.,Lonicera confusa DC or Lonicera fulvotomentosa Hsu et S.C.Cheng.Because of its low price and its similar appearance to LJF,it is easy to be imitated into LJF.If a certain amount of LF is mixed with LJF,it is difficult to detect with the naked eye and seriously affects the clinical efficacy.Therefore,rapid screening and quantitative analysis of adult LF in LJF is an important part of the raw material preparation process.Shuanghuanglian oral liquid is a LJF preparation,which is mainly composed of extracts of LJF,Scutellariae Radix and Forsythia Fructus.It has broad-spectrum antiviral,antibacterial,and immune function enhancement.It is currently one of the effective broad-spectrum antiviral drugs.In the pharmaceutical industry,shuanghuanglian oral liquid is usually sealed in containers made of various materials.Traditional chemical analysis methods will destroy the packaging of medicines and cause the loss and destruction of the tested samples.Therefore,a non-invasive detection method is needed for quality inspection of medicines after packaging.This article studies the feasibility of NIR spectroscopy in the non-invasive detection of bottled shuanghuanglian oral liquid,and this study also studies the factors that affect the accuracy of NIR spectroscopy,and the results prove that appropriate experiments design and chemometric algorithms can avoid interference factors in spectra measurement and improve measurement accuracy.This thesis conducts research on the above-mentioned problems,and the main research contents are as follows:1.In this study,FT-NIR spectroscopy and chemometrics are used for rapid analysis of adulterant LF in LJF.The powder of the pure Lonicerae Japonicae Flos,Lonicerae Flos and adulteration,and the corresponding extract solutions are prepared.FT-NIR spectra are modeled for comparison.SPA is used for characteristic bands selection;S-G,MSC,1st D and SNV are adopted for spectra preprocessing;PCA,and BPANN are employed as qualitative analysis method for screening whether or not containing adulteration;BPANN and PLS are used for quantitative analysis.The optimal results of screening and quantitative models are obtained from “S-G + MSC + SNV + BPANN” and “S-G + SNV + BPANN” of powder samples.It indicates that FT-NIR spectroscopy can provide a rapid and efficient tool for screening and quantitative analysis of adulterant Lonicerae Flos in Lonicerae Japonicae Flos.2.Based on the rapid detection of Lonicerae Japonicae Flos,this thesis studies the NIR spectroscopy non-invasive detection method of Lonicerae Japonicae Flos medicamentshuanghuanglian oral liquid.The NIR spectra method is an indirect measurement.It is necessary to establish a model with the reference value measured by the standard method to predict the content of the unknown sample.Therefore,UPLC method,photocolorimetric method and refraction methods were used to detect the contents of baicalin,total flavonoids and soluble solids in shuanghuanglian oral liquid.The experiment obtained 152 batches of sample data,which consisted of production samples and prepared samples obtained by freezedrying-dilution method to expand the range of sample variation.The methodology of UPLC was verified.The RSD value of the stability,precision and repeatability of baicalin were all less than 2%,the sample recovery was 99.4%,and the RSD was less than 2%,indicating that the stability of the sample is good,the precision of the instrument and the repeatability of the method are reliable.The established quantification is accurate and reliable,with good applicability,and can be used for the quantification of index components.3.In this study,NIR spectroscopy technology was applied to the non-invasive detection of Lonicerae Japonicae Flos medicament-bottled shuanghuanglian oral liquid,and a method to overcome the influence of ambient light and dark current of the instrument was proposed.NIR spectroscopy can be used as a non-invasive detection method,and the quality of the spectrum will directly affect the accuracy of the model measurement.The ambient light,instrument dark current,and changes in light source temperature will all affect the accuracy and stability of the spectra measurement.The chopping modulation technology modulates the light source,and the light source signal is loaded on a specific frequency to form a periodic signal.The modulated periodic signal can realize the separation of useful signal and random noise,effectively eliminating the influence of light source instability,ambient light and dark current of the instrument.In this study,baicalin,total flavonoids and soluble solid content were used as indicators to measure the quality of shuanghuanglian oral liquid,and Si PLS regression model was established with the NIR spectroscopy collected through the bottle.Compared with the unmodulated spectra,the RMSEP% of baicalin,total flavonoids and soluble solid content of the modulated spectra prediction model is reduced by 0.1055%,2.6955% and 2.1410%.Studies have shown that chopping modulation technology can filter out the influence of light source changes and dark current,and is an effective method to improve the accuracy of NIR spectroscopy.4.In order to reduce the influence of the difference of the oral liquid glass bottle and the measurement position shift on the quantitative analysis of NIR spectroscopy,and to improve the accuracy of the non-invasive quantitative analysis of the composition of the oral liquid,this paper proposes a spatial multi-dimensional spectra extraction method.Baicalin,total flavonoids and soluble solids are used as quality indicators for oral liquids,and PLS models are established for single-point and spatial multi-dimensional spectra,respectively.In order to ensure the validity of the model,the SPXY algorithm is applied to the division of calibration and validation sets,and MCCV is used to determine the number of latent variables.The RMSEP of the best single-point models are 0.8052 mg/m L(for baicalin),0.9526 mg/m L(for total flavonoids)and1.1097%(soluble solids),while the RMSEP of the best spatial multidimensional models are0.7953 mg /m L(for baicalin),0.7907 mg/m L(for total flavonoids)and 1.0037%(soluble solids).The results prove that the spatial multidimensional extraction method can improve the measurement accuracy of bottled oral liquid,and is an effective method to eliminate the uncertainty of measurement conditions.Based on NIR spectroscopy,this thesis carried out qualitative and quantitative detection of Lonicerae Japonicae Flos and Lonicerae Flos,and realized non-invasive detection of Lonicerae Japonicae Flos medicament-shuanghuanglian oral liquid,and adopted two experimental designs from different angles to improve the accuracy of NIR measurement.It proves that NIR spectroscopy is an effective method for quality control of Lonicerae Japonicae Flos herbs and medicaments.