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Study On The Methods Of Systematic Separation And Preparation Of Components From Moutan Cortex

Posted on:2014-08-02Degree:MasterType:Thesis
Country:ChinaCandidate:C M HanFull Text:PDF
GTID:2334330488999235Subject:Food Science
Abstract/Summary:PDF Full Text Request
Systematic understanding of components is an important role of traditional Chinese medicine(TCM)to be modernization,whose basic conditions are systemically composition separation.Chromatography technology,as an effective way of separation,make vital function step by step.Moutan Cortex as as the research object in this paper,meant to explore systematic separation based on chromatography technology for TCM,meanwhile provide basis and reference for others TCM separation,so as to form technical regulation of the scale preparation on industrial chromatography of TCM and improve the field's development.An ultra-performance liquid chromatography/quadrupole time-of-flight mass spectrometry(UPLC/Q-TOF-MS)method was established to characterize the compounds of Moutan Cortex,Thirteen compounds were identified from Moutan Cortex by analyzing the total ion current(TIC)chromatograms and MS fragmentation patterns,whose function was to have a preliminary acquaintance of Moutan Cortex.Based on the system solvent extraction,salting-out precipitation,ethanol precipitation and evaluation test,the pretreatment methods of Moutan Cortex determined by analysis of composition changes of TLC and HPLC technologies is that,which weakened the complexity of the samples,n-hexane,ethyl acetate extraction can effectively segment the extract from Moutan Cortex in the original pH conditions and enrichment of water phase conducted by Macroporous resin.The systematic TLC methods used to bolting chromatograph stationary phase and separation conditions,The results showed that silica gel is the suitable chromatograph stationary phase,Spots and separation degree in TLC,as index,determined n-hexane phase and water phase optimal elution solvents are n-hexane-acetone,chloroform-methanol respectively.The EtOAc part's suitable seperation mode is reversion.Fast separation of the n-hexane part,accomplished by Vacuum liquid chromatography(VLC).Step-gradient method forecast isolate and load mass studied utilized compounds of Frl.4 from n-hexane part,results show that under the condition of 0.10<Rf?0.65,step-gradient was appropriated to Frl.4 from w-hexane and six compounds separated up to 90%pxirity in practice with a 4*4 cm medium preparation liquid column(MPLC),in which load mass meet relationship of SiO2g?59.8Sg.It is avaliable separation that when two components' Rf between 0.10-0.30 in TLC and after four times development the?Rf?0.16.To sum up,the systematic separation with chromatography as the core and avariety other technologies assisted established by this study,which provides the reference basis for systemic components of TCM.
Keywords/Search Tags:Moutan Cortex, UPLC/Q-TOF-MS, preparative column, pre-treatment technology, chromatographic separation mode selection, predict of step-gradients
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