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A kind of separation and preparation method of wolfberry lutein HSCCC

A technology of wolfberry lutein and lutein, applied in the direction of organic chemistry, etc., to achieve the effect of reducing production cost, low price, and large seed particles

Inactive Publication Date: 2016-08-24
NINGXIA ACADEMY OF AGRI & FORESTRY SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, there is no report on the use of HSCCC technology to separate lutein from Lycium barbarum.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] The main steps of the separation and preparation method of wolfberry lutein HSCCC are as follows:

[0031] (1) Extraction: Weigh 10g of wolfberry fresh fruit, add methanol and tetrahydrofuran composite solvent to extract after grinding, the ratio of solid to liquid is 1:15, ultrasonic power is 300w, ultrasonic extraction is 30min, and the extract is obtained by filtration, and the filter residue is extracted twice according to the above operation. combined extracts;

[0032] The composite solvent is a composite solution of methanol and tetrahydrofuran with a volume ratio of 1:1, which contains 0.1% by mass and volume of BHT based on the total volume of the mixed solution.

[0033] (2) Concentration: Concentrate to 10 mL in the dark at 35 ° C to obtain a crude concentrate, add 100 mL of petroleum ether and 50 mL of 10% NaCl aqueous solution in a separatory funnel, wash the organic layer with 100 mL of pure water until colorless, and combine the organic layers , dehydrat...

Embodiment 2

[0039] The main steps of the separation and preparation method of wolfberry lutein HSCCC are as follows:

[0040] (1) extraction: with embodiment 1;

[0041] (2) Concentration: Concentrate to 11.25mL in the dark at 35°C to obtain a crude concentrate, add 90mL of petroleum ether and 70mL of 10% NaCl aqueous solution in a separatory funnel, wash the organic layer with 90mL of pure water until colorless, and combine the organic layer, dehydrated with anhydrous sodium sulfate, and concentrated to 11.25 mL to obtain a concentrate.

[0042] (3) Saponification: add 112mL10% KOH-methanol solution, fill with N 2 , Saponified at room temperature for 10 h under dark conditions to obtain a saponified solution.

[0043] (4) Elution and dissolution: add 100mL of petroleum ether and 70mL of 10% NaCl solution, wash the organic layer with pure water until neutral, avoid light, concentrate and evaporate to dryness, and dissolve the residue with 2mL of dichloromethane to obtain lutein dichloro...

Embodiment 3

[0046] The main steps of the separation and preparation method of wolfberry lutein HSCCC are as follows:

[0047] (1) extract with embodiment 1;

[0048] (2) Concentration: Concentrate to 10.5mL in the dark at 35°C to obtain a crude concentrate, add 126mL of petroleum ether and 84mL of 10% NaCl aqueous solution in a separatory funnel, wash the organic layer with 105mL of pure water until colorless, and combine the organic layer, dehydrated with anhydrous sodium sulfate, and concentrated to 10.5 mL to obtain a concentrate.

[0049] (3) Saponification: add 84mL10% KOH-methanol solution, fill with N 2 , Saponified at room temperature for 12h under dark conditions to obtain a saponified solution.

[0050] (4) Elution and dissolution: Add 95 mL of petroleum ether and 65 mL of 10% NaCl solution, wash the organic layer with pure water until neutral, avoid light, concentrate and evaporate to dryness, and dissolve the residue with 2 mL of dichloromethane to obtain a lutein dichlorome...

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Abstract

The invention discloses a method for preparing lycium barbarum lutein by HSCCC (high-speed countercurrent chromatography) separation. The method mainly comprises the following steps: grinding and extracting lycium barbarum berry, concentrating extract, saponifying, eluting and dissolving, and carrying out HSCCC separation to obtain a lycium barbarum lutein solution; concentrating, and freeze-drying to obtain a lutein pure product of which the purity is over 90.6 percent by means of HPLC analysis and detection. According to the method, a methanol and tetrahydrofuran composite solvent is adopted for ultrasonic extraction, and a saponification technology is combined and synergized with HSCCC, so that the problem that main carotinoid lutein and zeaxanthine in lycium barbarum belong to isomers and are difficult to separate can be successfully solved; autumn berry of lycium barbarum is utilized as a raw material, so that the production cost is greatly reduced, effective separation of lutein and zeaxanthine can be successfully realized by repeatedly regulating the solvent proportion in the counter-current chromatography separating and purifying phase, a high-purity lutein monomer can be obtained, and a new thought is provided to implementation of separating and purifying lutein from lycium barbarum and implementation of industrial production.

Description

technical field [0001] The invention belongs to the technical field of separation and purification, and in particular relates to a separation and preparation method of wolfberry lutein HSCCC. Background technique [0002] High-speed countercurrent chromatography (HSCCC for short) is a liquid-liquid distribution technology that can realize continuous and effective distribution and separation functions. It has the advantages of no sample loss, no pollution, high efficiency, rapid separation and large preparation volume. Since its invention, HSCCC technology has been continuously promoted and developed due to its unique separation advantages, and has been widely used in the separation of traditional Chinese medicine components, health food, biochemistry, bioengineering, natural product chemistry, organic synthesis and other fields. At present, my country's application of HSCCC technology is in the international leading position in the separation and purification of active ingre...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C403/24
Inventor 刘兰英曹有龙石志刚安巍
Owner NINGXIA ACADEMY OF AGRI & FORESTRY SCI
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