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Method for preparing lycium barbarum lutein by HSCCC (high-speed countercurrent chromatography) separation

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: 2015-03-25
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 Lycium barbarum Lutein HSCCC are as follows:

[0031] (1) Extraction: Weigh 10g of fresh wolfberry fruit, add methanol and tetrahydrofuran compound solvent to extract after grinding, material-to-liquid ratio 1:15, ultrasonic power 300w, ultrasonic extraction for 30min, and filter to obtain the extract. The filter residue is extracted twice according to the above operation. Combined extracts;

[0032] The composite solvent is a methanol and tetrahydrofuran composite solution 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 petroleum ether and 50 mL 10% NaCL aqueous solution to a separatory funnel, wash the organic layer with 100 mL pure water until colorless, and combine the organic layers , Dehydrated with anhydrous sodium sulfate, conc...

Embodiment 2

[0039] The main steps of the separation and preparation method of Lycium barbarum Lutein HSCCC are as follows:

[0040] (1) Extraction: same as Example 1;

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

[0042] (3) Saponification: add 112mL of 10% KOH-methanol solution, and fill with N 2 , Saponify at room temperature for 10h under dark conditions to obtain saponification liquid.

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

Embodiment 3

[0046] The main steps of the separation and preparation method of Lycium barbarum Lutein HSCCC are as follows:

[0047] (1) Extract the same as in Example 1;

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

[0049] (3) Saponification: Add 84mL of 10% KOH-methanol solution, and fill with N 2 , Saponify at room temperature for 12h under dark conditions to obtain saponification liquid.

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

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PUM

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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 particularly relates to a method for separating and preparing Lycium barbarum Lutein HSCCC. Background technique [0002] High-speed countercurrent chromatography (HSCCC) is a liquid-liquid distribution technology that can achieve continuous and effective distribution and separation functions. It has the advantages of no loss of samples, no pollution, high efficiency, rapidity and large volume separation. Since the invention of HSCCC technology, due to its unique separation advantages, it has been continuously promoted and developed. It has been widely used in the separation of 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 a leading position in the world in the separation and purification of active ingredients of natural medicin...

Claims

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Application Information

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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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