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Solanesol extracting and preparing process

A solanesol and low-carbon alcohol technology, applied in the field of solanesol, can solve the problems of low total yield, uneconomical operation cost, and environmental pollution, and achieve low cost, significant economic and social benefits

Inactive Publication Date: 2006-08-02
EAST CHINA UNIV OF SCI & TECH +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The main disadvantages of this process are: 1. The total yield is low, and the silica gel column with too low content of solanesol will affect the reutilization rate of silica gel, and the operation cost is uneconomical; the solanesol content higher than 70-75% is obtained by solvent method It is difficult to obtain after two to three recrystallizations, even if it can be obtained by solvent method, the yield is lower; 2. The silica gel chromatography process is easily affected by solvent purity, column packing conditions, etc., and the fluctuation of process conditions is difficult to control; 3. Pollution to the environment , silica gel column chromatography, due to the difficulty of regeneration, it is generally thrown away directly to pollute the environment, and the cost of silica gel consumed per month amounts to tens of thousands of yuan

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Dissolve 50 grams of crude extract of tobacco leaves containing 14% solanesol in 50 ml of n-hexane under stirring, and set aside after the dissolution is complete. Take 50ml of ethanol and 5g of sodium hydroxide, mix them evenly, add them to the above mixture, heat to an inner temperature of 60°C and stir for saponification for 3 hours, cool to room temperature, and filter the reaction solution for later use.

[0020] About 300 grams of the processed macroporous adsorption resin HZ-802 (handled according to the conventional treatment method of ion exchange resin and adsorption resin) is packed into a glass column with a diameter of 5 cm and a length of 100 cm. The lower end is a polytetrafluoroethylene piston. The sand core at the upper end of the piston is No. 2 sand core. Pass the above mixture into a glass column at room temperature, and pass it through in about 10 minutes, then use a) 2000ml of ethanol; b) 10000ml of acetone: ethanol = 1:1 mixture; c) 2000ml of acet...

Embodiment 2

[0022] Dissolve 50 grams of crude extract of tobacco leaves containing 14% solanesol in 50 ml of n-hexane under stirring, and set aside after the dissolution is complete. Take 50ml of methanol and 5g of sodium hydroxide, mix them evenly, add them to the above mixture, heat to an internal temperature of 60°C and stir for saponification for 3 hours, cool to room temperature, and filter the reaction solution for later use.

[0023] About 300 grams of the processed macroporous adsorption resin HZ-803 (treated according to the conventional treatment method of ion exchange resin and adsorption resin) is packed into a glass column with a diameter of 5 cm and a length of 100 cm, and the lower end is a polytetrafluoroethylene piston. The sand core at the upper end of the piston is No. 2 sand core. Pass the above mixture into a glass column at room temperature, and pass it through in about 10 minutes, then use a) 2000ml of ethanol; b) 10000ml of acetone: ethanol = 1:1 mixture; c) 2000ml...

Embodiment 3

[0025] Dissolve 50 grams of crude tobacco leaf extract containing 14% solanesol in 50 ml of n-hexane under stirring, and set aside after the dissolution is complete. Take 50ml of ethanol and 7g of potassium hydroxide and mix them evenly, then add them to the above mixture, heat to an internal temperature of 60°C and stir for saponification reaction for 3 hours, cool to room temperature and filter the reaction solution for later use.

[0026] About 300 grams of the processed macroporous adsorption resin HZ-816 (treated according to the conventional treatment method of ion exchange resin and adsorption resin) is packed into a glass column with a diameter of 5 cm and a length of 100 cm, and the lower end is a polytetrafluoroethylene piston. The sand core at the upper end of the piston is No. 2 sand core. Pass the above mixture into a glass column at room temperature, and pass it through in about 10 minutes, then wash it with a) 2000ml of methanol; b) 10000ml of acetone:methanol=1...

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Abstract

The process of extracting and preparing high purity solanesol from tobacco extractum includes: dissolving crude tobacco extractum in alkane solvent, saponifying under alkali alcoholate condition for 3 hr, filtering the reaction product, adsorbing the filtrate with macroporous resin, eluting with low toxicity mixed lower ketone and lower alcohol solvent, rotary evaporating the eluted solution to recover solvent, and decompression vacuum drying to obtain solanesol in the purity of 90-95 %. The said process has simple operation, reusable solvent, low cost and no pollution, and may be used in industrial production of solanesol in the purity over 90 %.

Description

technical field [0001] The invention relates to a biochemical separation technology, in particular to a method for extracting and preparing high-purity solanesol from tobacco leaf extract by adsorption-chromatography Background technique [0002] Solanesol is a polyisoprenyl alcohol, its pure product is a white powdery solid with a melting point of 41°C. Solanesol is a long-chain fatty alcohol with weak polarity and is easily soluble in organic solvents. Solanesol mainly exists in flue-cured tobacco leaves, and also contains a small amount of solanesol in potato leaves and mulberry leaves. Solanesol can be extracted and separated from tobacco leaves as a raw material for the synthesis of vitamin K and coenzyme Q10. It is also an important constituent structure of many drugs, and studies have shown that the effects of many drugs are significantly enhanced after the introduction of the solanesol structure. It is the side chain of coenzyme Q10 (heart...

Claims

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Application Information

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IPC IPC(8): C07C29/74C07C33/02
Inventor 徐环昕江邦和季华沈永雷刘坐镇
Owner EAST CHINA UNIV OF SCI & TECH
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