The Reaearch About The Technique Of Solvent Sublation Applied In Separation And Purification Of Effective Constituent From Natural Products Solanum Rostratum And Glycyrrhiza Uralensis

The accuracy and reproducibility of analytical results and the sensitivity of analytical methods are mainly dependent on the sample pretreatment technique if the detecting instrument is stable during the analysis.Now there is a great tendency to develop the sample pretreatment technique with high speed,large amount,easy operation,low cost,low dosage of organic solvent,green and environmentally-friendly.In recent years,solvent sublation has been applied in many fields such as the separation of metal ions,chiral compounds,effective constituent in natural products,the analysis of organic pollutants,because of its high separation efficiency,high concentration factor,low consumption of organic reagent and so on.In this paper,the application of solvent sublation on the separation and purification of active constituent in natural products was studied in detail,and the obtained main results were as follows:1.The method of "Aqueous two-phase flotation(ATPF)-HSCCC-low column temperature semi-preparative HPLC" was established for the separation and purification of four flavonol glycosides in Solanum rostratum Dunal.Firstly,fraction 1 and fraction 2 were obtained with the flotation efficiency of 90.51%and 92.07%,respectively,under the optimal conditions of ATPF;Secondly the flotation product was separated by HSCCC and fraction 1 and fraction 2 were obtained with purities of 96.03%and 94.27%,respectively,by the HPLC analysis,then the fraction 1 and fraction 2 were identified by LC/MS and NMR with the result that fraction 1 was quercetin 3-O-β-D-galactopyranoside and fraction 2 was the mixture of three compounds;Thirdly,fraction 2 was further separated by low column temperature semi-preparative HPLC and kaempferol 3-O-β-D-glucopyranoside,3’-O-methy lquercetin 3-O-β-D-galactopyranoside and 3’-O-methylquercetin 3-O-β-D-glucopyranoside in fraction 2 were obtained with the purities of 96.70%,95.33%and 99.92%,respectively.2.The method of "Three-liquid-phase flotation(TLPF)-Semi-preparative HPLC" was established for the separation and purification of five bioactive substances in Glycyrrhiza uralensis Fisch.Firstly,liquiritin apioside,liquiritin,glycyrrhizic acid,semilicoisoflavone B and licoisoflavone B were obtained with the flotation efficiency of 91.24%,94.23%,88.04%,94.67%and 96.44%,respectively,in the optimal conditions of TLPF;Then the flotation products in middle phase and upper phase were separated by semi-preparative HPLC and the five compounds were acquired with the purities of 83.10%、96.45%、93.11%、93.58%and 96.20%,respectively.