| Induced phase separation is a novel liquid-liquid extraction method for separating different substances by means of phase transformation by adding inducer in homogeneous solvent.Compared with the traditional liquid-liquid extraction,induced phase separation has the advantages of simple operation,high flux,low solvent consumption,and the toxicity of acetonitrile is small,which accords with the requirement of green chemistry.In this paper,the solvent characteristics of the induced phase separation system are explained preliminarily and used in the separation and extraction of the active components from Chinese medicinal herbs.The main contents of the thesis are as follows:In the first chapter,the development of induced phase separation and the research progress of the micro-properties of the induced phase separation solvent are reviewed,and the structure of the solvatochromic dye probe and application in the study of solvent polarity are introduced.The separation and extraction methods of active components of Chinese herbal medicine were introduced.In the second chapter,the changes of the micro-properties of acetonitrile-water and acetone-water in the solvents system of the induced phase separation were studied.The influence of the increase of water content on the displacement and peak strength of the bond in the solvent and the Raman displacement of the characteristic bond before and after the salt-induced phase separation were studied by Raman spectroscopy.With the increase of water content,the frequency shift amplitude and displacement direction of characteristic peak of hydrogen bond,which is between organic solvents and water,are different.The Raman characteristic peaks,which is between acetonitrile and water,are shifted to low wave numbers(red shift),and the frequency shift amplitude is small;the Raman characteristic peaks,which is between acetone and water,are shifted to Takanami number(blue Shift),and the frequency shift amplitude is larger.The strength of the Raman characteristic peaks between organic solvents(acetonitrile and acetone)and water is increasing.By using NaCI,(NH4)ZCO3 and Na2CO3 as inducer,the CN telescopic vibration characteristic peak of acetonitrile was moved to the Takanami number while the characteristic peak of the CO telescopic vibration characteristic peak of acetone after the phase separation moved to the low wave number.The solution polarity was characterized by ET,and the change of the solution ET before and after the inducted phase separation was determined by ultraviolet visible spectrum.When most inorganic salts(except for ammonium carbonate and barium chloride)are inducers,the ET value of the organic phase after the phase separation is between the pure organic phase and the mixed solution,which indicates that the polarity of the organic phase after phase separation is between the pure organic and the mixed solution polarity of water and organic.Comparing the degree of changes,hydrogen bonding is an important factor affecting the polarity of solution,but it is not the only factor,while other factors,such as intermolecular force,affect the polarity of solution.In the third part,induced phase separation method is applied to the separation and purification of alkaloids from Coptis chinensis.The ratio,type and volume of the separation solvent system,quality and kind of inducer and extraction time were optimized.When ammonium sulfate was inducer,the initial extract powder was extracted by acetonitrile-water,alkaloids can transfer to acetonitrile effectively while others were transferred to the aqueous phase.After drying the acetonitrile phase,the alkaloids content in the dry slag jatrorrhizine was 6.38%,coptisine was 11.64%,palmatine was 7.44%,and berberine was 25.4%.Its content is much higher than raw materials(jatrorrhizine 1.74%,coptisine 2.98%,palmatine 1.83%,berberine 0.0381%).Compared with the traditional liquid-liquid extraction and filling column separation,the induced phase separation method is more environmentally friendly and can be used in the purification of alkaloids preparation.In the fourth chapter,solvent induced phase separation was applied to separate flavonoids glycosides and aglycones of different pharmacological activities in Scutellaria baicalensis Georgi.The extraction solvents and separation solvents of the sample solution were optimized,by establishing the HPLC-MS fingerprint of Scutellaria baicalensis Georgi,the main chemical constituents were analyzed,and the seven kinds of components of Scutellaria baicalensis Georgi were confirmed,and Baicalein and Baicalin were used as the index components by solvent-induced phase separation to separate flavonoids from Scutellaria baicalensis Georgi to explore the conditions for maximum separation of glycosides and glycosides.The optimum separation capacity of flavonoids and glycosides from Scutellaria baicalensis Georgi was determined by 6 g as the inducer of acetonitrile-water solvent system and chloroform. |
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