Establishment Of Novel Green Extraction Method And Application In Effective And Toxic Compounds Of Traditional Chinese Medicine

The chemical composition of traditional Chinese medicine is complex,and the traditional extraction methods have the disadvantages of low extraction efficiency,long extraction time,and the use of toxic reagents as extraction solvents.Therefore,it is particularly important to study new extraction methods of traditional Chinese medicine.In this study,a new green extraction method was established,various factors affecting extraction efficiency were optimized,and systematic methodological verification was performed,which can efficiently,quickly and sensitively detect the active and harmful ingredients in traditional Chinese medicine.The specific research content is as follows:1. The main active components in Hawthorn leaves possess various biological activities such as anti-inflammatory,antioxidant,and hypolipidemic effects.Therefore,it is needed to develop an effective and reliable extraction method to extract these active compounds from Hawthorn leaves.In this study,the microwave-assisted reaction and extraction(MARE)combined with ultra-high performance liquid chromatography with ultraviolet detector method was established to extract and determine the polyphenolic compounds in Hawthorn leaves.The solid reagent aqueous solutions were applied as extraction solvents,preventing the use of organic solvents.The target analytes were identified by quadrupole time-of-flight tandem mass spectrometry.Several experimental parameters that can significantly affect the extraction efficiency were evaluated and optimized.The optimal conditions were as follows:0.1 g of sodium carbonate was used as solid reagent,the amount of sodium borate was set at 0.01 g,extraction time was 10 min,extraction temperature was set at50 ~oC,p H value was adjusted at 7.The validation experiments demonstrated that the method had high sensitivity with the limits of detection in the range of 26.5-37.7ng/m L.The average recoveries were ranged from 80.22 to 93.27%.In this work,the proposed MARE method was successfully applied to extract and determine polyphenolic compounds in Hawthorn leaf samples.Compared with other reported methods,the present method was faster,greener,and more sensitive.2. A simple,rapid and environmentally friendly method named effervescence-assisted matrix solid-phase dispersion(EA-MSPD)was investigated for the extraction of four coumarins(esculin,esculetin,fraxin and fraxetin)from Crotex fraxini(C.fraxini).In this study,an effervescent tablet containing carbon dioxide sources(100 mg sodium bicarbonate and 200 mg sodium dihydrogenphosphate)and an adsorbent(25 mg benzo-15-crown-5)was prepared.The effervescent tablet was dissolved into an aqueous solution,and as a consequence of the effervescence reaction,carbon dioxide was generated,thus making the sample better a dispersion of the extraction solvent(100 m M sodium dodecyl sulfate).The variables that influenced the extraction efficiency included effervescent salts,extraction solvents and crown ether.These values were represented using ultra-high-performance liquid chromatography.Good linearity was exhibited by coefficients of determination all equal to 1,limits of detection ranging from 1.62 to 3.83 ng/m L and limits of quantification ranging from5.39 to 12.76 ng/m L.The recoveries ranged from 91.37 to 100.29%with relative standard deviations of 0.57-4.58%under optimized conditions.In this work,the proposed EA-MSPD method was successfully applied to extract and identify four coumarins in C.fraxini.Compared with previously reported methods,the method examined herein was faster,greener and more sensitive.3. A microwave (MW)treatment assisted with miniaturized solid phase extraction(mini-SPE)method was developed for the detection of the pesticides compounds in the Dendrobium officinale Kimura et Migo using ultrahigh performance liquid chromatography coupled with quadrupole time-of-flight mass spectrometry(UHPLC-Q-TOF/MS).This study presented the fabrication of activated carbon from hawthorn leaf.Activated carbons were made by different chemical agent activation coupled with MW treatment and carbonisation of the hawthorn leaf under certain pressure,various concentration of chemical activating agent,MW temperatures and time.The optimal experimental conditions were determined as:chemical activating agent concentrated hydrochloric acid,concentrated hydrochloric acid concentration 10:1,MW time 30 min,and MW temperature 150.The method revealed that a satisfactory linearity(r~2?0.9927)was obtained.The limits of detection(LODs)ranged from 0.08 to 1.35 ng/m L for the seven pesticides according to the optimum experimental conditions.The accuracy of the current mini-SPE method was studied by recovery in Dendrobium officinale Kimura et Migo,yielding values81.17-106.12%.The mini-SPE method coupled with UHPLC-Q-TOF/MS and activated carbons from hawthorn leaf by microwave-induced concentrated hydrochloric acid activation were successfully applied for the determination and extraction of the pesticides compounds in Dendrobium officinale Kimura et Migo.