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Process for purifying solanesol from tobacco leaf extract

A technology of solanesol and tobacco leaves, which is applied to the field of purifying solanesol from tobacco leaf extract and the preparation of intermediates, and can solve the problems of product purity and quality failing to meet requirements, complicated process, and insignificant purity improvement.

Inactive Publication Date: 2007-04-25
郑亚津
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] In the prior art, the purification of solanesol from tobacco leaf extract mainly includes solvent crystallization, column chromatography separation and molecular distillation, etc. Solvent crystallization, such as CN1115751A patent, is to extract fatty alkane, add alcohol and alkali saponification, and use alcohol and ketone mixed solvent Treat crystallization, the crystallization can reach 90%, but the solvent consumption is large, the cost is high, and the quality is not required
[0004] Column chromatographic separation method such as CN1345711A patent uses adsorption chromatography and gel permeation chromatography to carry out chromatographic separation and crystallization purification, but the requirements for raw materials are relatively high (more than 70%), and two column chromatographic separations are required. The process is complicated and the flow required There are many matches, and it is difficult to control in industrial applications
[0005] Molecular distillation method, such as CN1115751A patent, uses a molecular distillation and short-path distillation technology to process tobacco leaf extract in stages to obtain tobacco absolute and solanesol, but the purification of solanesol by this technology is very limited, and the purity improvement is not obvious
[0006] The technology of purifying solanesol from tobacco leaf extract that can be applied to the synthesis of coenzyme Q10 still has some defects, such as high cost, large solvent consumption, and product purity and quality that cannot meet the requirements, etc., which limit large-scale industrial production. application

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Weigh 100kg of tobacco leaf extract with a solanesol content of 14.5% and add it to the saponification tank, start the agitator, add 100kg of 20% lye at an even speed within 30 minutes, keep warm at 60°C for three hours, and add 500kg of n-hexane after saponification The alkane was stirred and extracted three times, and the n-hexane layer was collected under reduced pressure to recover the n-hexane to obtain 71kg of n-hexane extract. The liquid extract was kept at 40°C and the flow rate was controlled at 0.5 liters / min. The concentration is controlled below 1-10 Pa to obtain 38kg of light phase transparent tobacco leaf absolute and heavy phase solanesol. Solanesol is dissolved in n-hexane and added to a silica gel chromatographic column. : 20 ratio for mobile phase elution, collect the high-purity solanesol segment, and desolventize to obtain 9.1kg of high-purity solanesol, keep the high-purity solanesol at 40°C and control the flow rate to 0.1 liter / min and pour it into...

Embodiment 2

[0030] Weigh 100kg of Yinye extract with a content of 16.7% into the saponification tank, start the agitator, add 100kg of 15% lye at an even speed within 30 minutes, keep warm at 55°C for three hours, and add 500kg after saponification The n-pentane was stirred and extracted three times, and the n-pentane layer was collected under reduced pressure to recover the n-pentane to obtain 75kg of n-pentane extract. The liquid extract was kept at 40°C and the flow rate was controlled at 0.5 liters / min. The temperature is 150°C, the vacuum degree is controlled below 1-10 Pa, and the light phase transparent tobacco leaf absolute and the heavy phase solanesol 43kg are obtained, and the solanesol is dissolved in n-pentane and added to a silica gel column, and n-pentane and acetone The mixed solvent was used as mobile phase elution at a ratio of 100:15, and the high-purity solanesol segment was collected and desolvated to obtain 9.6kg of high-purity solanesol. The high-purity solanesol was...

Embodiment 3

[0032] Weigh 100kg of tobacco leaf extract with a solanesol content of 13.2% and add it to the saponification tank, start the agitator, add 100kg of 25% lye at an even speed within 30 minutes, keep warm at 65°C for three hours, and add 500kg of petroleum oil after saponification The ether was stirred and extracted three times, and the petroleum ether layer was collected under reduced pressure to recover the petroleum ether to obtain 65 kg of petroleum ether extract. The liquid extract was kept at 40°C and the flow rate was controlled at 0.5 liters / min. The concentration is controlled below 1-10 Pa to obtain 39kg of light phase transparent tobacco leaf absolute and heavy phase solanesol. Solanesol is dissolved in petroleum ether and added to a silica gel chromatographic column, and the mixed solvent of petroleum ether and methanol is used at a ratio of 100:8. The proportion is used for mobile phase elution, and the high-purity solanesol segment is collected and desolvated to obt...

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PUM

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Abstract

The invention discloses a preparing method of solanesol, which comprises the following steps: adopting tobacco leaf with solanesol content at 13-17% as raw material; saponifying through alkaline solution; extracting through saturated paraffin; decompressing extract to recycle the solvent; proceeding once molecular distillation for fluid extract; separating the dissolved solanesol through column chromatography; collecting solanesol segment by segment; desolventizing the solanesol; distilling to purity; obtaining the product with purity more than 95%. The invention can separate high-effect component of different tobaccos, which saves cost with high safety.

Description

technical field [0001] The invention relates to an intermediate preparation technology in the field of fine chemical industry, in particular to a method for purifying solanesol from tobacco leaf extract. Background technique [0002] The English name of solanesol is Salanesol; its molecular formula is C45-H740, and its pure product is white or light yellow solid powder; it is easily soluble in organic solvents such as ether, acetone and hydrocarbons. Solanesol is a natural product that widely exists in higher plants, mammals and microorganisms. The content of solanesol in leaves of tobacco and other Solanaceae plants is prominent, especially in tobacco leaves as high as 0.3-3%. Solanesol is an important raw material for drug synthesis and an irreplaceable key intermediate of ubiquinone drugs, that is, the side chain of coenzyme Q10 and vitamin K2. An important intermediate of cancer drugs, widely used in medicine. [0003] In the prior art, the ...

Claims

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Application Information

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IPC IPC(8): C07C29/74C07C33/02
Inventor 郑亚津陈红辉
Owner 郑亚津
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