Studies On Preparation Of Solenesol

Solanesol is an important medical intermediate, and is widely used in medicine. Because solenesol is a kind of terpene alcohol with a long hydrocarbon group, it is difficult to synthesis. So it is obtained mainly from vegetable leaves particularly from tobacco leaves now. The planting area and the annual yield of tobacco in our country are No.1 in the world, that is to say our nation has the abundant tobacco resource. This paper mainly studied the method of purifying solenesol from tobacco extractum by recrystallization, and established an processing line to produce high-purity solenesol which is suitable to industrialization. And we studied the structure of the production, finding that the processing line had no effect on solenesol structure,and the purity of production can meet the synthesis requirement. The main research contents and the results as follows:Firstly, we studied the terms and conditions of quantitative analysis of solenesol by HPLC. The results showed that solenesol could be perfectly separate from other substance by using Diamonsil ODS-C₁₈( 5μm Column4.6mmid×250mm ) as analytical column, acetonitrile– isopropyl alcohol (3/2, v/v) as mobile phase, 30℃as column temperature, 1mL/min as the flow rate, DAD uv-detector as the detector, 203nm as the detecting wavelength, and the retention time of solenesol is 17min. The experiment of precision degree measured the RSD of the method was 0.62%, which showed that the method had good repeatability;the experiment of add-on and recoverying the standard measured the standard deviation of the method was 4.32 and the CV was 4.341, which showed the method had high recovery rate; the linear rage of the method was 0.80-8.0 mg/mL.The content of solenesol, the saponification value and the acide value in tobacco extractum were analysised and the saponifical technics of the tobacco extractum was studied though single factor and normal experiments. The analysis and the study showed that the content of solenesol in tobacco extractum is 12.4%, the saponification value and the acide value in tobacco extractum are 74.80 mgKOH/g extractum and 11.87mgKOH/g extractum respectively; the requirement of alkali for the saponification of tobacco extractum was 89.76 mgKOH/g extractum. The preferable condition of the saponification was putting the extractum into 0.3mol/L NaOH-EtOH, on the temperature of 70℃saponifying 2 hours. And under the conditions the aponification rate was over 97.4%.The technological conditions of producing 70% solenesol product were resesrched. And the results showed the best conditions were using acetonitrile as the crystal solvent, 1: 20 (g:mL) as the weight of material ratioing the volume of crystal solvent , 40% as the use level of absorbent charcoal, 80% as the density of ethanol used as cleaning agent, 4℃ad the crystal temperature. And under the perfect condition the content of solenesol in the production is 70.06%, and the recovery ratio of solenesol is 71.54%.The processing technology of producing the production in which the content of solenesol is above 90% was researched, finding that the solution which was saturated by CaCl₂ can remove the foreign substance with minor polarity very well. The conditions of producing the ideal production were forecasted thong the models of ANN and GA. The experimental result and the forecasted result were compared, finding that the models of ANN and GA can be used to lead the experiments.The experimental data were treated comprehensively, finding the ideal conditions are 1:5 (g:mL) as the weight of material ratioing the volume of solution which was saturated by CaCl₂, 67℃as the treating temperiture , 12h as the time of rflux exraction flowsheet, 64℃as the temperature of rflux exraction flowsheet, -4℃as the crystal temperature of removing foreign substance, -22℃as the crystal temperature of mother liquid. And under the perfect condition the content of solenesol in the production is 92.62%, and the recovery ratio of solenesol is 60.74%.Lastly the structure of the product was rearched, both the IR atlas and the MS atlas show that the new technology of producing solenesol product had no effect on the structure of solnesol.