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Lutein crystal preparing process from marigold flower

A technology of marigold flowers and lutein, applied in the direction of organic chemistry, can solve the problems of difficult recovery, high viscosity, low product content, etc., and achieve the effects of simple process operation, high extraction yield, and low separation difficulty.

Inactive Publication Date: 2003-08-20
海宁凤鸣叶绿素有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

There have been reports abroad on the extraction, separation, and purification of lutein crystals from marigold flowers. However, if the process is applied to actual production, there are problems such as difficulties in the separation of lutein crystals, large amounts of organic solvents used, and difficulties in recovery.
For example: U.S. Patent US 5382714, the amount of organic solvent used in saponification is large, the separation of lutein is difficult, the product content is low, and the recrystallization uses a toxic dichloromethane / methanol combination solvent, which is not conducive to the application of the product in food and medicine; US 5648564, saponification with 45% alkali propylene glycol solution, because the viscosity of propylene glycol is high, there is also the problem of difficult separation, and the propylene glycol in the waste liquid is extremely difficult to recycle, and it is easy to cause pollution to the environment; and US6262284 uses tetrahydrofuran and alkali alcohol solution in Simultaneously carry out extraction and saponification at room temperature, and finally recover the organic solvent, but the amount of organic solvent is too large, the energy and solvent consumption are too large, and because under alkaline conditions, higher fatty acid salts and alcohols are prone to esterification reactions to generate higher fats Ester colloids and lutein are precipitated together, so lutein crystals are also difficult to separate and purify

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] Extraction, saponification, separation, washing, drying: dry marigold flower granules 2kg, n-hexane 2L, continuous leaching at 60°C for 5-6 times, combine the extracts and vacuum recover n-hexane to a volume of 500ml-600ml; heat up to 56°C , under stirring, add 40g of sodium hydroxide, the weight ratio of sodium hydroxide and water is 1:5; control the temperature at 50°C to 60°C, stir and saponify for 3 hours to 10 hours, and use thin layer chromatography to show saponification reaction After completion, let stand and cool down; dilute the saponification reaction product with 100ml of deionized water at a temperature of 60°C, and then perform centrifugation; wash the obtained lutein crystals with deionized water at 70°C until the eluate is neutral; and drying at room temperature for 72 hours to obtain 35.5 g of lutein crystals with a content of 83% and a total extraction rate of lutein of 85.2%.

[0016] Recrystallization: Dissolve lutein crystals (10g, 83%) in 200ml te...

Embodiment 2

[0018] Extraction, saponification, separation, washing, drying: dry marigold flower granules 2kg, petroleum ether 2L, continuously extract 5-6 times at 60°C, combine the extracts to vacuum recover petroleum ether to a volume of 500ml-600ml; after heating to 56°C , under stirring, add 60g of sodium hydroxide, the weight ratio of sodium hydroxide and water is 1:5, control the temperature at 50°C to 60°C, stir and saponify for 3 hours to 10 hours, and use thin layer chromatography to show saponification reaction After completion, let stand and cool down; dilute the saponification reaction product with 100ml of deionized water at a temperature of 60°C, and then perform centrifugation; wash the collected lutein crystals with deionized water at 70°C until the eluate is neutral; After drying under vacuum and room temperature for 72 hours, 37.3 g of lutein crystals with a content of 75.6% were obtained, and the total extraction rate of lutein was 75.10%.

[0019] Recrystallization: Di...

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PUM

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Abstract

The present invention is the lutein crystal preparing process from marigold flower. Lutein ester is first extracted from marigold flower with non-polar solvent under heating condition and then saponified with alkali solution in stirring and heating condition; and the saponified product is diluted with deionized water and separated, washed and vacuum dried. After that, the obtained lutein crystal is re-crystallized in three-component solvent of tetrahydrofuran, deionized water and normal hexane or petroleum ether; and the lutein crystal is suction filtered, washed and vacuum dried. The present invention has low-toxicity solvent in small amount used, simple technological process, high extraction, rate, and high product purity. The product of the present invention may be used widely as feed coloring additive and food coloring agent and in medicine and health care article.

Description

technical field [0001] The patent of the present invention relates to a method for preparing lutein crystals from marigold flowers. Background technique [0002] Lutein is a kind of carotenoid, which is very high in dark green leafy vegetables such as cabbage, kale and spinach, as well as flowers such as calendula and marigold. Lutein is one of the most effective color-enhancing additives among carotenoids, which can improve the appearance, color and internal quality of livestock and poultry products when used in livestock and poultry feed; natural lutein is also an excellent antioxidant, used as food Additives have a good effect on preventing a series of diseases caused by organ aging, such as preventing vision loss and blindness caused by senile macular degeneration. [0003] Taking marigold flowers as raw material to extract lutein, the domestic existing technology is limited to the production of pasty liquid and paste resin, such as Qingdao University Science and Techno...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C403/24
Inventor 徐水明沈凤明
Owner 海宁凤鸣叶绿素有限公司
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