Study On The Extraction And Separation Of Solanesol From Inferior And Waste Tobacco Leaves

In China, tobacco yield and planted area, which have reached 4500,000—5000,000 ton and 1300,000 hektare, are the most great in the world. Nearly 25%of it was wasted. Solanesol in tobacco leaves is an important intermediatematerial of medicine. It is difficult to separate and purify Solanesol from naturalmaterials, and the technology to purifying Solanesol was monopolized byJapan for a long period, most enterprises in China could only manufacture crudeSolanesol product with low added value, which content of Solanesol was below20%. Therefore, many researchers have focused on the extraction and purifyingtechnology of Solanesol from inferior and waste tobacco leaves in recentyears.In this dissertation, extraction and purifying technology of Solanesolfrom inferior and waste tobacco leaves was studied thoroughly, and the resultswere obtained as below1. The determination methods of TLC and HPLC were established. Thedeveloping solvent was petroleum ether- ethyl acetate (4:1,v/v) in TLCAcetaldol sulphuric acid ethanol solution was color agent, developed color at100℃for 5min, wavelength was 620nm, slit size was 1.25×1.25, linearization coefficient sx=3. The mobile phase was methanol-ethanol (1:1,v/v) in HPLC,chromatographic column was KromasiL ODS C18, 5μL, 250×4.6mm;wavelength was 215nm; column temperature was 30℃. The method of TLC islow-cost, quick, easy-operate and suitable for on-line analysis, whereas themethod of HPLC is more accurate.2. PA was the best by comparing effect of different entrainersduring the extraction of SFC. Optimized parameters were obtained throughorthogonal experiment, ratio of solid:liquis was 5:1 (M/V), extraction vesselpressure was 20Mpa, extraction vessel temperature was 30℃, separationvesselâ… pressure was 7Mpa, separation vesselâ… temperature was 35℃,separation vesselâ…¡pressure was 4Mpa, separation vesselâ…¡temperature was30^C, flux of CO₂ was 20L/h, extraction time was 3h. The yield and purity ofsolanesol was 5.15% and 10.95% under this conditions,3. The extraction solvent and extraction methods were studied. It wasbetter by circumfluence extraction with solvent PA. Through orthogonalexperiment, Optimized parameters were obtained: The extraction time was 3h,the extraction temperature was 40℃, and the material: solvent was 1:8. Underthus conditions, the yield was high, the stability was good, and it could beoperated easily.4. Saponification process conditions were optimized by orthogonalexperiment. Take solvent YH as Saponification media, the temperature was50℃, the time was 3h, the amount of NaOH was 1/40 of the material, the amount of Solanesol after saponification increased by 0.72 times under thusconditions,5. Column chromatography conditions of Solanesol were optimized byorthogonal experiment.The sorbent was silica gel at activity grade 2, ethanolwas eluant, and filled in Column by dry method. Under those conditions, thepurity and recovery are high and respectively reach 59.7% and 73.5%.6. Crude Solaneso was purified by re-crystallization. The solvent andcrystal conditions were studied. Results showed that YHL was the best crystalsolvent, and the crystal process were as below: YHL by 12 times amountdissolve the crude Solaneso, standing for 5 h at -2℃, filtrated, thenrecrystallization. The average purity was 97.0%, the max purity was 98.2%, therecovery reached up to 83.7%. This process was simple, short-term, low-cost,easy-operate, and high purity and recovery, it is a better method at present.