Solanesol is an important secondary metabolite in Nicotiana tabacum. Distribution of solanesol in Nicotiana tabacum was investigated by High Performance Liquid Chromatography （HPLC） method. The quantitative distribu...Solanesol is an important secondary metabolite in Nicotiana tabacum. Distribution of solanesol in Nicotiana tabacum was investigated by High Performance Liquid Chromatography （HPLC） method. The quantitative distribution of solanesol in various organs and tissues of N. tabacum showed that solanesol content, obviously different in all organs, was 6.8, 18.3, 27.5, 45.8, and 68.0 times higher in leaves than that in the stalks, flowers, seeds, fruits and roots, respectively. The contents of solanesol in various parts of leaf, stalk and flower were determined. The content of solanesol in top leaf, middle leaf and bottom leaf gradually decreased （6.124, 5.813 and 5.687 mg.g^-1, respectively） and the content of solanesol in various leaf-parts （leaf apex, leaf middle and leaf base） also gradually decreased. The content of solanesol in top stalk was 1.19 times and 1.92 times higher than that in the middle stalk and the bottom stalk, respectively. The content of solanesol in various tissues of stalk （epidermis, cortex and stele） dramatically decreased. The sepal contained higher concentration of solanesol （1.192 mg·g^-1） compared to any other parts in flower. The study will provide the base data for the regulation and control of solanesol, moreover, it will provide the scientific evidences for the rational development and utilization of N. tabacum resources.展开更多
The saponification （30%） were studied in this work conditions of crude solanesol The results showed the content of solanesol arrived to 41.9%; the optimal conditions of solanesol saponification were the saponificati...The saponification （30%） were studied in this work conditions of crude solanesol The results showed the content of solanesol arrived to 41.9%; the optimal conditions of solanesol saponification were the saponification time of 3 hours, the saponification temperature about 45℃, amount of 2.5g NaOH and amount of 30mL C2H5OH. NEWTON-LAPUSON method was applied to iterate. The correlative equations provide an effective basis for further research of refining solanesol.展开更多
A separation integrated technology for isolating refined solanesol from tobacco extracts was provided. Some experimental installations applied in the separation integrated technology were designed. The experimental in...A separation integrated technology for isolating refined solanesol from tobacco extracts was provided. Some experimental installations applied in the separation integrated technology were designed. The experimental installations included saponification and extraction installation, cryogenic centrifugation crystallization installation and continuous midium pressure column chromatography separation installation In the paper, a separation integrated technology route was designed： saponification and extraction-crystallization - silica gel column chromatography-recrystallization. Finally, refined solanesol （-95.5%） was successfully got. The new method featured shorter experimental times, as well as lower solvent consumption, compared with the conventional extraction methods. So it showed great potential for efficient sample preparation and large-scale industrial application in the near future.展开更多
In order to extract solanesol from potato stems and leaves more effectively and improve the extraction rate of solanesol, the same batch of potato stems and leaves harvested from Guyuan, Ningxia was selected as a rese...In order to extract solanesol from potato stems and leaves more effectively and improve the extraction rate of solanesol, the same batch of potato stems and leaves harvested from Guyuan, Ningxia was selected as a research object, cell wall of potato stems and leaves was broken by enzymolysis with cellulase and high- speed shearing, and then reflux-extracted with 95% ethanol. Solanesol content was determined by HPLC, and extract yield was calculated. Extract yield and solanesol extraction rate was used as an index for comparison of difference between the 2 wall-breaking methods, so as to select the optimal wall-breaking method. The results showed that enzymolysis with cellulase exhibited extraction rate and extract yield of solanesol of 91.38% and 8.02%, respectively, which were better than those under high-speed shear emulsification technique. The enzymolysis wall-breaking method has the advantages of simple operation and strong feasibility.展开更多
Trimethoxybenzoyloxysolanesylamide（8） was first synthesized from solanesol in four steps. Thus, solanesyl bromide（5） prepared by the reaction of solanesol（4） and PBr3 was reacted with potassium phthalimide to gi...Trimethoxybenzoyloxysolanesylamide（8） was first synthesized from solanesol in four steps. Thus, solanesyl bromide（5） prepared by the reaction of solanesol（4） and PBr3 was reacted with potassium phthalimide to give N-solanesylphthalimide（6）, which was refluxed with N2H4·H2O in 95%EtOH to give solanesylamine（7）. Compound 7 was then reacted with 3,4,5-trimethoxybenzoyloxyl chloride to give the title compound. Its structure has been confirmed by IR, 1H NMR, MS and elemental analysis.展开更多
Solanesyl bromide(Ⅱ) was reacted with diethanolamine to give solanesyl diethanolamine(Ⅲ) which was acylated with 3,4,5 trimethoxybenzoyl chloride, acetic anhydride, benzoyl chloride and cinnamyl chloride to give N,N...Solanesyl bromide(Ⅱ) was reacted with diethanolamine to give solanesyl diethanolamine(Ⅲ) which was acylated with 3,4,5 trimethoxybenzoyl chloride, acetic anhydride, benzoyl chloride and cinnamyl chloride to give N,N di[(3,4,5 trimethoxybenzoyloxy)ethyl]solanesylamine(Ⅳ), N,N di[(acetyloxy)ethyl] solanesylamine(Ⅴ), N,N di[(benzoyloxy)ethyl]solanesylamine(Ⅵ), N,N di[(cinnyloxy)ethyl]solanesylamine(Ⅶ) respectively. The structures of compounds Ⅲ～Ⅶ were confirmed by IR, 1H NMR, MS and elemental analysis.展开更多
Extraction and determination method of solanesol in waste tobacco leaves by combination of(ultrasonic) extraction and high performance liquid chromatography(HPLC) was demonstrated.Ultrasonic(extraction) showed advanta...Extraction and determination method of solanesol in waste tobacco leaves by combination of(ultrasonic) extraction and high performance liquid chromatography(HPLC) was demonstrated.Ultrasonic(extraction) showed advantage over the other methods.Thereby the conditions of ultrasonic extraction were(optimized).The results show that extraction yield is the highest under 80 kHz for 20 min with 80% ethanol at a ratio of V(liquid)/m(solid)=10 mL/g.展开更多
基金This paper was supported by Special fund of technological innovation talents in Harbin city, China (No. 2006RFQXN003)
文摘Solanesol is an important secondary metabolite in Nicotiana tabacum. Distribution of solanesol in Nicotiana tabacum was investigated by High Performance Liquid Chromatography （HPLC） method. The quantitative distribution of solanesol in various organs and tissues of N. tabacum showed that solanesol content, obviously different in all organs, was 6.8, 18.3, 27.5, 45.8, and 68.0 times higher in leaves than that in the stalks, flowers, seeds, fruits and roots, respectively. The contents of solanesol in various parts of leaf, stalk and flower were determined. The content of solanesol in top leaf, middle leaf and bottom leaf gradually decreased （6.124, 5.813 and 5.687 mg.g^-1, respectively） and the content of solanesol in various leaf-parts （leaf apex, leaf middle and leaf base） also gradually decreased. The content of solanesol in top stalk was 1.19 times and 1.92 times higher than that in the middle stalk and the bottom stalk, respectively. The content of solanesol in various tissues of stalk （epidermis, cortex and stele） dramatically decreased. The sepal contained higher concentration of solanesol （1.192 mg·g^-1） compared to any other parts in flower. The study will provide the base data for the regulation and control of solanesol, moreover, it will provide the scientific evidences for the rational development and utilization of N. tabacum resources.
文摘The saponification （30%） were studied in this work conditions of crude solanesol The results showed the content of solanesol arrived to 41.9%; the optimal conditions of solanesol saponification were the saponification time of 3 hours, the saponification temperature about 45℃, amount of 2.5g NaOH and amount of 30mL C2H5OH. NEWTON-LAPUSON method was applied to iterate. The correlative equations provide an effective basis for further research of refining solanesol.
文摘A separation integrated technology for isolating refined solanesol from tobacco extracts was provided. Some experimental installations applied in the separation integrated technology were designed. The experimental installations included saponification and extraction installation, cryogenic centrifugation crystallization installation and continuous midium pressure column chromatography separation installation In the paper, a separation integrated technology route was designed： saponification and extraction-crystallization - silica gel column chromatography-recrystallization. Finally, refined solanesol （-95.5%） was successfully got. The new method featured shorter experimental times, as well as lower solvent consumption, compared with the conventional extraction methods. So it showed great potential for efficient sample preparation and large-scale industrial application in the near future.
基金Supported by Ningxia Agricultural Comprehensive Development Demonstration Project of Integration of Potato Green High-yielding and Mechanized Operation Techniques in 2015(NTKJ2016-09-03)
文摘In order to extract solanesol from potato stems and leaves more effectively and improve the extraction rate of solanesol, the same batch of potato stems and leaves harvested from Guyuan, Ningxia was selected as a research object, cell wall of potato stems and leaves was broken by enzymolysis with cellulase and high- speed shearing, and then reflux-extracted with 95% ethanol. Solanesol content was determined by HPLC, and extract yield was calculated. Extract yield and solanesol extraction rate was used as an index for comparison of difference between the 2 wall-breaking methods, so as to select the optimal wall-breaking method. The results showed that enzymolysis with cellulase exhibited extraction rate and extract yield of solanesol of 91.38% and 8.02%, respectively, which were better than those under high-speed shear emulsification technique. The enzymolysis wall-breaking method has the advantages of simple operation and strong feasibility.
文摘Trimethoxybenzoyloxysolanesylamide（8） was first synthesized from solanesol in four steps. Thus, solanesyl bromide（5） prepared by the reaction of solanesol（4） and PBr3 was reacted with potassium phthalimide to give N-solanesylphthalimide（6）, which was refluxed with N2H4·H2O in 95%EtOH to give solanesylamine（7）. Compound 7 was then reacted with 3,4,5-trimethoxybenzoyloxyl chloride to give the title compound. Its structure has been confirmed by IR, 1H NMR, MS and elemental analysis.
文摘Solanesyl bromide(Ⅱ) was reacted with diethanolamine to give solanesyl diethanolamine(Ⅲ) which was acylated with 3,4,5 trimethoxybenzoyl chloride, acetic anhydride, benzoyl chloride and cinnamyl chloride to give N,N di[(3,4,5 trimethoxybenzoyloxy)ethyl]solanesylamine(Ⅳ), N,N di[(acetyloxy)ethyl] solanesylamine(Ⅴ), N,N di[(benzoyloxy)ethyl]solanesylamine(Ⅵ), N,N di[(cinnyloxy)ethyl]solanesylamine(Ⅶ) respectively. The structures of compounds Ⅲ～Ⅶ were confirmed by IR, 1H NMR, MS and elemental analysis.
文摘Extraction and determination method of solanesol in waste tobacco leaves by combination of(ultrasonic) extraction and high performance liquid chromatography(HPLC) was demonstrated.Ultrasonic(extraction) showed advantage over the other methods.Thereby the conditions of ultrasonic extraction were(optimized).The results show that extraction yield is the highest under 80 kHz for 20 min with 80% ethanol at a ratio of V(liquid)/m(solid)=10 mL/g.
