Extraction Of Solanesol From Tobacco Leaves By Different Extraction Methods And Its Characterization

Solanesol is one of the most important terpenoid compounds in tobacco.It has a certain effect on flue gas and is an important intermediate for the synthesis of coenzyme Q10 and vitamin K2.Tobacco polysaccharides are not only actively affect the taste and flavor of cigarettes,but also play a key role in the moisture retentivity.Effects of ultrasonic extraction and smashing tissue extraction of solanesol in low-grade tobacco leaves were studied in this work.The purified solanesol was got,then its thermal properties was tested.Tobacco polysaccharides were extracted from filtrate produced by water washing pretreatment and moisture retentivity of it were studied.Study results as follows: 1.Ultrasonic technology and smashing tissue extraction were applied to extraction of solanesol from low-grade flue-cured tobacco leaves in this work.The influence of different organic solvent,granularity,liquid-solid ratio,extraction time,ultrasonic power,extraction temperature and extraction times were studied in extraction of solanesol by single factor design using ultrasonic technology.The Box-Behnken design and response surface methodology were employed to optimize the ultrasound-assisted extraction of solanesol from tobacco leaves with the aim to maximize their extraction yield.The optimum ultrasonic extraction parameters were as follows: ultrasonic power 100 W,liquid-solid ratio 15: 1(m L/g),extraction temperature 45 ℃ and extraction time 69 min.Single factor experiment was applied to invest the effects of liquid-solid ratio,extraction time,voltage and times on extraction yield of solanesol by smashing tissue extraction.Box-Behnken design and response surface methodology were employed to optimize the smashing tissue extraction of solanesol from tobacco leaves with the aim to maximize their extraction yield.The optimum smashing tissue extraction parameters were as follows: liquid-solid ratio 17:1(m L/g),the voltage 112 V and extraction time 108 s.Under the optimal extraction conditions,yield of solanesol were 2.64% and 2.78% respectively.The latter extraction rate was slightly higher than the fomer.2.Cost of two extraction methods were analyzed.Cost of ultrasound-assisted extraction was higher than smashing tissue extraction for the same weight of solanesol.Some large-scale experiments were conducted based on condition of optimum smashing tissue extraction parameters and the results suggested that the industrialization of solanesol from tobacco leaves was feasible.3.Saponification,column chromatography separation and crystallization three methods were used to separate and purificate above sample.The purity of solanesol was 38.06% after saponification,and the yield was 94.63%.Orthogonal experiment design was applied to optimizate factors of column chromatography separation.The results showed that the optimum parameters were as follows: urea and silica gel mass ratio 1: 1(g: g),eluent volume 50: 1 and inlet sample quantity 0.200 g.Under this condition,the purity of solanesol was 59.87% after saponification,and the yield was 75.20%.The mixed solvent of methanol-acetone-n-hexane(1: 1: 2,V: V: V)was used as the primary crystallization reagent and methanol was used in recrystallization.Purity of solanesol was 93.63% after saponification,and the yield was 67.50%.Isolated compounds were identified solanesol by high resolution mass spectrometry and infrared spectroscopy.4.Thermal properties of solanesol was test by themogravimetry-derivative themogravimetry-differential scanning calorimetry(TG-DTG-DSC)and pyrolysis-gas chromatography-mass spectrometry(Py-GC-MS).Solanesol had a severe degradation from 209.8~359.8 ℃ with mass loss 75.29% and second severe degradation from 479.8~559.8 ℃ with mass loss 16.24%.The thermal cracking behavior of solanesol was studied under simulated cigarette conditions.The results showed that 73 compounds were solvated at the temperature of 300,600 and 900 ℃,including flavorous substances D-Limonene,3-hydroxy-2-Butanone and 3,7-dimethyl-6-octen-1-Oformate.From the perspective of the influence of solanesol on cigarette smoke,the volatile products of pyrolysis have a positive contribution to flue gas.5.Tobacco polysaccharides were extracted from filtrate produced by water washing pretreatment.Sevage method was used to purificate polysaccharides sample.Polysaccharide extraction yield 0.708% was determinate by phenol-sulfuric acid method.Moisture retentivity was studied and the results showed that cut tobacco moisture ability with tobacco polysaccharides was stronger than with the samples of propylene glycol under the environment of low relative humidity.Tobacco polysaccharides had moisture-proof effect at a moderately high humidity.