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
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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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