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Method for preparing high-purity solanesol by using crude cigarette paste

A solanesol and high-purity technology, which is applied in the field of preparing high-purity solanesol by using crude tobacco extract, can solve the problems of numerous types of organic solvents, difficulty in solvent recovery, and difficulty in operation, and achieves easy industrial production and high degree of mechanical application. , The effect of the overall process is simple

Inactive Publication Date: 2013-03-13
GUANGDONG FOOD IND INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

For example, the application number is 200510111768.7 and the application number is 200410067949.X and other patent application publications. Resin column chromatography is used in the disclosed methods, and there are many types of reagents, and the operation is difficult.
In addition, the application number is 200410040400.1. In the method disclosed in the patent application publication specification, cyclohexane, acetone-alcohol and other solvents have been used. Although the saponification process has been used to improve the yield and content, there are many types of organic solvents, resulting in solvent recovery. difficulty

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Add 5 grams of sodium hydroxide and 500 grams of 30% (V / V) ethanol-water mixed solvent to 100 grams of crude tobacco paste, and hydrolyze and saponify at 60 ° C for 6 hours to obtain saponified products. Add 10 grams of calcium chloride to the saponification product, stir to dissolve, separate the upper layer solution while hot, and concentrate the dry solvent of the lower layer viscous product under reduced pressure to obtain 95 grams of oily substance. The oily substance was heated and dissolved with 1100 g of 95% ethanol solution, cooled to 30°C and filtered to obtain a filtrate, and the filtrate was concentrated to dryness to obtain 42 g of ethanol extract. The ethanol extract was first dissolved with 129 grams of petroleum ether, then extracted with 214 grams of 50% (V / V) ethanol-water mixed solvent, the petroleum ether layer was separated, and the petroleum ether was concentrated and recovered to obtain 21 grams of yellow viscous, yellow viscous The thick matter w...

Embodiment 2

[0030] Add 6 grams of sodium hydroxide and 700 grams of 40% (V / V) ethanol-water mixed solvent to 100 grams of crude tobacco paste, and hydrolyze and saponify at 70 ° C for 7 hours to obtain a saponified product. Add 13 grams of calcium chloride to the saponification product, stir to dissolve, separate the upper layer solution while hot, and concentrate the dry solvent of the lower layer viscous product under reduced pressure to obtain 93 grams of dark brown oil. The oily substance was heated and dissolved with 1200 g of 97% ethanol solution, cooled to 35° C. and filtered to obtain a filtrate, and the filtrate was concentrated to dryness to obtain 40 g of ethanol extract. The ethanol extract was first dissolved in 140 grams of petroleum ether, then extracted with 240 grams of 60% (V / V) ethanol-water mixed solvent, the petroleum ether layer was separated, and the petroleum ether was concentrated and recovered to obtain 19 grams of yellow sticky substance. Dissolve the yellow vis...

Embodiment 3

[0032] Add 7 grams of potassium hydroxide and 800 grams of 50% (V / V) ethanol-water mixed solvent to 100 grams of crude tobacco paste, and hydrolyze and saponify at 90 ° C for 10 hours to obtain a saponified product. Add 15 grams of calcium chloride to the saponification product, stir and dissolve, separate the upper layer solution while hot, and concentrate the dry solvent of the lower layer viscous product under reduced pressure to obtain 91 grams of oily matter. The oily substance was heated and dissolved with 1300 g of 95% ethanol solution, cooled to 30°C and filtered to obtain a filtrate, and the filtrate was concentrated to dryness to obtain 43 g of ethanol extract. The ethanol extract was first dissolved with 200 grams of petroleum ether, then extracted with 400 grams of 70% (V / V) ethanol-water mixed solvent, the petroleum ether layer was separated, and the petroleum ether was concentrated and recovered to obtain 20 grams of yellow sticky substance. The yellow viscous ma...

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PUM

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Abstract

The invention discloses a method for preparing high-purity solanesol by using crude cigarette paste. The method comprises the following steps: (1) adding alkali and a mixed solvent of alcohol water into crude cigarette paste, and hydrolyzing and saponifying at 60-90 DEG C for 6-10 h to obtain saponification products; (2) adding a metal salt precipitating agent into the saponification products, stirring for dissolution, separating out an upper solution while hot, and conducting decompression condensation on a lower dope to obtain an oil substance; (3) dissolving the oil substance by ethanol solution, heating the oil substance, cooling to 30-40 DEG C, filtering to obtain a filtrate, and concentrating the filtrate to obtain an ethanol extract; (4) dissolving the ethanol extract with petroleum ether, then extracting with the mixed solvent of alcohol and water to separate out a petroleum ether layer, and concentrating and recovering petroleum ether to obtain a yellow dope; and (5) decolorizing the yellow dope, and recrystallizing to obtain solanesol with purity higher than 90%. The process provided by the invention has advantages of high degree of solvent nesting, low production cost, high yield and purity, and easiness for realization of industrialization production.

Description

technical field [0001] The invention relates to a method for extracting solanesol, in particular to a method for preparing high-purity solanesol by using crude tobacco paste. Background technique [0002] Solanesol is a polyisoprenyl alcohol with the molecular formula H(CH 2 C(CH 3 )CHCH 2 ) 9 OH, the relative molecular weight is 631, the pure product is a white powdery solid, and the melting point is 41°C. Solanesol is a long-chain fatty alcohol with weak polarity, easily soluble in organic solvents, insoluble in water, and has certain solubility in alcohol solvents. As an important pharmaceutical intermediate, solanesol is the synthesis of coenzyme Q 10 and vitamin K 2 In addition, in the field of medicine, its downstream products also have the effect of preventing and treating cardiovascular and cerebrovascular diseases. The existence of solanesol in tobacco leaves is mainly in two forms: free state and esterified state, of which the free state solanesol accounts f...

Claims

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Application Information

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IPC IPC(8): C07C33/02C07C27/02C07C29/76
Inventor 杜阳吉王三永李春荣
Owner GUANGDONG FOOD IND INST