Method for preparing high-content xanthophyll crystal from Calendula officinalis extract

A technology for lutein and extract, applied in the field of preparing high-content lutein crystals, can solve the problems of high cost, difficult separation, large amount of organic solvent, etc., and achieves reduced preparation cost, less damage and loss, and less environmental pollution Effect

Active Publication Date: 2009-05-20
黑龙江省嘉宝生物技术开发有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The method (CN1436774A) for preparing lutein crystals from marigolds developed by Zhejiang Haining Fengming Co., Ltd., the method uses tetrahydrofuran, petroleum ether and other mixed solvents to recrystallize to obtain pure lutein, the extraction rate is below 60%, and the saponification reaction time is relatively short. Long, complex process, high cost, and difficult solvent recovery
[0005] U.S. Patent US 5382714, the amount of organic solvent used in saponification is large, the separat

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Weigh 40g of Calendula officinalis extract (content is 150g / kg) in a 100ml round-bottomed flask, add 5g of sodium hydroxide and 10g of methanol successively under electromagnetic stirring, add 0.2g of vitamin C, bathe in 60°C water, fill with nitrogen protection, and react for 2.5 hour, add 20 parts of 5°C deionized water to dilute, centrifuge, collect the filter residue, wash the filter residue with 5°C deionized water until the pH value of the effluent liquid is 6.5, and vacuum dry to obtain crude lutein. The crude lutein was washed twice with 10 parts of n-hexane each, and centrifuged, and the lutein crystals were dissolved in methylene chloride at room temperature to obtain a saturated solution, and 0.2 times of n-hexane was added dropwise to the saturated solution until turbidity appeared , centrifuged. The freeze-drying time is 20 hours. Obtain 5.6g of 98% lutein crystals. The effective conversion rate was 91.5%.

Embodiment 2

[0032] Weigh 250g of Calendula officinalis extract (content is 150g / kg) in a 500ml round-bottomed flask, add 16g of potassium hydroxide and 34g of methanol in turn under electromagnetic stirring, add 1.2g of vitamin E, put in a water bath at 60°C, fill with nitrogen protection, and react for 2.5 Add 20 parts of 5°C deionized water for dilution, centrifuge, collect the filter residue, wash the filter residue with 5°C deionized water until the pH value of the effluent liquid is 6.7, and vacuum dry to obtain crude lutein. Wash the crude lutein twice with 10 parts of n-hexane, centrifuge, dissolve the lutein crystals in dichloromethane at room temperature to obtain a saturated solution, add 0.3 times of n-hexane dropwise to the saturated solution until it becomes turbid , centrifuged. The freeze-drying time is 20 hours. 35.5 g of 97.7% lutein crystals were obtained. The effective conversion rate was 92.5%.

Embodiment 3

[0034] Weigh 100g of Calendula officinalis extract (content is 150g / kg) into a 250ml round-bottomed flask, under electromagnetic stirring, potassium hydroxide 6g, ethanol 22g, vitamin E 0.5g, 60 ℃ water bath, nitrogen protection, reaction 2.5 Add 20 parts of 5°C deionized water for dilution, centrifuge, collect the filter residue, wash the filter residue with 5°C deionized water until the pH value of the effluent liquid is 7.0, and vacuum dry to obtain crude lutein. Wash the crude lutein twice with 8 parts of n-hexane, centrifuge, dissolve the lutein crystals in dichloromethane at room temperature to obtain a saturated solution, add 0.3 times of n-hexane dropwise to the saturated solution until it becomes turbid , centrifuged. The freeze-drying time is 20 hours. 14.3 g of 97.5% lutein crystals were obtained. The effective conversion rate was 93.0%.

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Abstract

The invention relates to a method for preparing high-content lutein crystal with a pot marigold extract, wherein, the pot marigold extract is firstly dissolved in an alkaline alcohol solution, and then an antioxidant and inert gas shielding are added for carrying out a saponification reaction. The pot marigold extract is changed into lutein in a free state, and the lutein is diluted with deionized water and washed till the pH value of the lutein is 6.5 to 7.0. The lutein goes through vacuum drying to obtain a crude product of the lutein. The crude product is recrystallized by a non-polar or weak-polar organic solvent, and centrifugally filtered, cooled and dried to obtain a product with purity of more than 98 percent. The method has simple production technology, small toxic amount of the solvents, less consumption and easy recovery as well as easy realization of industrialized production. The product can be applied to the fields of food colorants, food additives, pharmaceutical health products and the like in a safe and efficient manner.

Description

(1) Technical field [0001] The invention relates to a method for preparing high-content lutein crystals from calendula officinalis extract. (2) Background technology [0002] Carotenoids are natural pigments that widely exist in nature. So far, more than 700 kinds of carotenoids have been discovered and purified. Lutein is a kind of carotenoids. It has been found that lutein mainly includes the following Aspects of functions: ① Use its coloring property as feed and food additives; ② As a stabilizer for other substances; ③ Prevent macular degeneration in the elderly; ④ Anti-cancer effects; ⑤ Prevent and treat cardiovascular and cerebrovascular diseases. [0003] Lutein is a major carotenoid in green leafy vegetables and other plants. There are two forms of lutein in plants, free form and lutein ester; free lutein can be directly absorbed and utilized by the human body, while Lutein esters must be hydrolyzed into free lutein in the body before they can be absorbed. Therefore,...

Claims

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Application Information

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IPC IPC(8): C07C403/24A61K36/28
Inventor 王宝根赵志刚王丹
Owner 黑龙江省嘉宝生物技术开发有限公司
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