Study On New Techniques For Extraction And Detection Of Active Ingredients And Toxic Components In Common Chinese Medicine

The chemical components of traditional Chinese medicine are very complex in nature,including active ingredients,as well as ineffective and toxic components.Therefore,the extraction of active ingredients and the screening of toxic components are crucial to the safety and medical efficacy of traditional Chinese medicine.In this study,we established green micro-extraction methods coupled with novel detection methods to improve the extraction efficiency,selectivity and sensitivity of the whole analysis process.The main research contents are as follows:1.A rapid,simple and efficient sample extraction method based on micro-matrix-solid-phase dispersion was applied to the extraction of polyphenols from pomegranate peel.Carbon molecular sieve was firstly used as adsorbent to improve extraction efficiency in micro-matrix-solid-phase dispersion.Results showed that the proposed method was of good linearity(coefficient of determination r~2>0.990),the limit of detection(LOD)was as low as 3.2 ng/mL,which demonstrated nice reliability and high sensitivity of this approach.2.A rapid,effective process,which involves microwave-assisted extraction and dispersive micro-solid phase extraction,has been proposed for the extraction and detection of 6 mycotoxins in peach seed,milk powder,corn flour and beer samples.The results indicated good linearity(r?0.9982),low limits of detection and satisfactory spiked recoveries(84.27-104.96%).3.A simple and effective method of miniaturized solid-phase extraction was developed for the simultaneous purification and enrichment of macrolide antibiotics from honey and skim milk.Mesoporous MCM-41 silica was synthesized and used as sorbent in the procedure.Under the optimized condition,satisfactory linearity,acceptable precision,high sensitivity and good recoveries were obtained.4.Dispersive micro solid phase extraction combined with ultrahigh-performance liquid chromatography coupled with quadrupole time-of-flight tandem mass spectrometry method was established to extract and determine sudan dyes and their metabolites in real samples.The crown ether microfunctionalized multi-walled carbon nanotubes was applied as the sorbent in this procedure.The validation data showed that the limits of detection were in the range of 0.084-13.13?g/kg,the mean recoveries were ranged from 80.15 to 103.58%for six samples.Compared with other published methods,the proposed method was more effective,time-saving and eco-friendly.5.A fast,simple,and cost-effective miniaturized solid-phase extraction method using calixarenes as adsorbent was developed for the micro-extraction of cyanazine,simazine,atrazine,and propazine from complex samples(honey and milk).Under optimal conditions,the linear range was 6-600 ng/mL with the coefficients of determination from 0.9943 to 0.9998.The limits of detection for the four triazines were 0.01-0.04 ng/mL.6.In this work,electrochemistry(EC)coupled to mass spectrometry(MS)is used as a tool for the simulation of the oxidative pathway of phenolic acids in Danshen.The results obtained by EC were compared with rat microsomes and reported methods in vivo studies.Both methods showed good agreement with the data from EC/MS.7.This study aimed at developing an efficient analytical protocol for the determination of Hawthorn active ingredient and their electrochemical products.Compared to rat liver microsomal incubations and previously identified in vivo metabolites,the result shows the high potential of EC/MS as a fast analytical tool in the prediction of metabolic transformation.