Studies On "Green" Extracting And Isolation Technology Of Chimonanthus Salicifolius Hu. And Its Chemical Constituents

Chimonanthus Salicifolius Hu.used as a traditional Chinese medicine of the civilian She minority is vested in Calycanthus,and has been commonly applied to remedy in the epigastric fullness,chronic gastritis,stomach-ache,gastrectasia and pantothenic acid.Three coumarins compounds of the antiinflammatory components,the 6-methyl-7-methoxylcoumarin(Compound 1),6,7-dimethoxycoumarin,(Compound 2)and 6,7,8-trimethoxycoumarin(Compound 3)were extrac-ted firstly from this medicinal plant.The 6-methyl-7-methoxylcoumarin was used to drug intermediates synthesis.Scoparone,the another name of 6,7-dimethoxycoumarin,possesses the specific action as follows:anti-allergic,immunosuppressive,vasodilation,lipid lowering,antioxid-ant,anti-inflammatory,antiasthmatic action,and it might have potential for application in the treatment of neurodegenerative diseases,Parkinson disease and diabetes mellitus.The 6,7,8-trimethoxycoumarin demons-trates significant activity against the inflammatory,HIV.We researched the "green" extraction process of the coumarin from the limb of Chimonanthus Salicifolius Hu.The extraction methods were sumarized as follows:1.Ionic liquids(ILs)have been considered as "environmenttally friendly" solvents and the 1-Butyl-3-methylimidazolium tetrafluoroborate ILUAE have remarkable effects on the extraction efficiency.The optimum values of factors were 1.9 h(extraction time),1.9 ml(IL dosage),13.0 ml(solid-liquid ratio)per 1g for 6,7-dimethoxycoumarin,(Compound 2)and 6,7,8-trimethoxycoumarin(Compound 3).The productivity of two compounds is 0.21 mg·g-1 and 0.62 mg·g-1 respectively by HPLC.This method offers a high-speed,convenient and environmentally friendly method of obtaining natural products.2.For researching the effective extraction methods of coumarin from Chimonan thus Salicifolius Hu.,the surface active agent was applied for the extraction of coumarin coupoumds from this medicinal plant.we anasyzed factors and three levels through application of Design Expert 7.1.3 Response Surface’s software on base of single factor.Two highly productive(Compound 2)and 6,7,8-trimethoxycoumarin(Compound 3)were separated from Chimonanthus salicifolius Hu.for the first time.The optimum values of factors were 1.4 h(extraction time),23 g·L-1(SDS dosage),25 ml(solid-liquid ratio)per 1 g for 6,7-dimethoxycoumarin,(Compound 2)and 6,7,8-trimethoxycoumarin(Compound 3)and the productivity of two compounds is 0.21 mg·g-1 and 0.70 mg·g-1 respectively by analysis result and experiment.3.High-speed counter-current chromatography(HSCCC)was used for the separation of coumarins compounds from the crude sample of Chimonanthus salicifolius Hu.in this studies.The solvent system,n-heptane-ethyl acetate-methanol-water(0.8:1.2:0.8:1.2,v/v),was selected as the fluid system in fractional extraction.A few of major coumarins including 6-methyl-7-methoxylcoumarin(Compound 1),6,7-dimethoxycoumarin,(Compound 2)and 6,7,8-trimethoxycoumarin(Compound 3)were obtained in an one-step separation.The productivity of three compounds is 150 mg·g-1,40 mg·g-1 and 10 mg·g-1 respectively.The purity 98%of target compounds was exceeded entirely after HPLC analysis.4.The solvent System,chloroform:methyl alcohol:water(1:1:1,v/v),was chosen for the extraction of coumarin compounds from Chimonanthus salicifolius Hu..The upper phase was mainly composed of water.In contrast,the primary component of lower phases was chloroform.Most of the target compounds was positioned at the lower phases.The content of total coumarin was 96%,which contained 6-methyl-7-methoxylcoumarin(Compound 1),6,7-dimethoxycoumarin,(Compound 2)and 6,7,8-trimethoxycoumarin(Compound 3)and the productivity of coumarin compounds was 319 mg·g-1.