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Preparation and stabilization of high-purity xanthophyll ester and method for removing pollutant thereof

A high-purity technology for lutein esters, applied in the field of phytochemistry, can solve the problems of poor stability, low yield of lutein esters, and high residual amount of heavy metal substances, so as to increase the content, avoid solvent crossover, and solve the problem of poor yield. high effect

Active Publication Date: 2009-07-22
INNOBIO CORP LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] In order to solve the problems of low lutein ester yield, high pesticide residues and heavy metal residues, and poor stability in the prior art

Method used

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  • Preparation and stabilization of high-purity xanthophyll ester and method for removing pollutant thereof
  • Preparation and stabilization of high-purity xanthophyll ester and method for removing pollutant thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] Weigh 100 g of marigold flower grains with a total ester content of 4.1 wt % and mix with 1000 g of acetone, heat and stir at 70° C. for 0.5 hour and then filter to obtain an acetone extract. Add 50g of EDTA sodium salt and 50g of white clay to the acetone extract, stir at 70°C for 0.5h, filter, and remove the acetone in a vacuum to obtain the concentrate (the dissolved residue of the concentrate must be controlled to be less than 3% of its mass). Add tert-butanol 10 times the mass of the concentrate, stir and dissolve at 50°C for 1 hour, then slowly cool the solution to 10°C.

[0027] After the solution was placed at 10° C. for 18 hours, it was filtered to obtain a filter cake, which was mixed with 15 times the mass of methanol and washed with stirring. The washing times were three times, each time using methanol 5 times the mass of the solid. Add 0.5g of antioxidant vitamin E to the solid after fully washing with methanol, and dry it at 30°C for 24 hours to obtain 15g...

Embodiment 2

[0029] Weigh 100 g of marigold flower grains with a total ester content of 4.1 wt%, mix with 2000 g of acetone, heat and stir at 40° C. for 1.0 hour and then filter to obtain an acetone extract. Add 15g of EDTA sodium salt, 15g of attapulgite and 8g of white clay to the acetone extract, stir at 60°C for 1 hour, filter, and remove the acetone in a vacuum to obtain a concentrate (the dissolved residue of the concentrate must be less than 3% of its mass). Add isopropanol 3 times the mass of the concentrate, stir and dissolve at 40°C for 2h, then cool the solution slowly to 5°C.

[0030] After the solution was placed at 5° C. for 12 hours, it was filtered to obtain a filter cake, which was mixed with 9 times the mass of methanol and washed with stirring. The number of washings was three times, each time with 3 times the mass of solid methanol. Add 0.4g of the antioxidant vitamin C sodium salt to the solid after fully washing with methanol, and dry it at 40°C for 16 hours to obtain...

Embodiment 3

[0032] Weigh 120 g of marigold flower grains with a total ester content of 4.8 wt % and mix with 1500 g of n-butane, heat and stir at 20° C. for 5 hours and then filter to obtain n-butane extract. Add 12g of clay to the n-butane extract, stir at 30°C for 4h, filter, and remove the n-butane in a vacuum to obtain a concentrate (controlling the dissolved residue of the concentrate must be less than 3% of its mass). Add n-butanol with 1 times the mass of the concentrate, stir and dissolve at 20°C for 5h, then cool the solution slowly to 0°C.

[0033] After the solution was placed at 0°C for 10 hours, it was filtered to obtain a filter cake, which was mixed with ethanol 3 times its mass and washed with stirring. The washing times were three times, each time with ethanol 1 times the mass of the solid. Add 0.8g of antioxidant vitamin E to the solid washed with ethanol, and dry it at 45°C for 10 hours to obtain 13g of the product, which contains 90% of the mass percentage of lutein es...

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Abstract

The invention relates to method for preparing and stabilizing high-purity lutein ester and removing pollutants thereof; at temperature of 20 DEG C to 70 DEG C, the particles of marigold flowers are dissolved in normal butane or acetone, stirred for 0.5h to 5h and filtered to obtain an extraction solution; an adsorbing agent is added into the extraction solution, stirred for 0.5h to 5h at temperature of 20 DEG C to 70 DEG C and filtered; a mother solution is collected and dried in vacuum, thus obtaining a concentrated substance. The concentrated substance is dissolved in isopropanol or butyl alcohol, stirred for 0.5h to 5h at temperature of 20 DEG C to 70 DEG C and slowly cooled to -10 DEG C to 10 DEG C after forming an even solution, and then filtered after 6 to 18 hours; the filter mass is added with an antioxidant after being washed by lower alcohol, and then dried to remove the lower alcohol, and thus the high-purity lutein ester is finally obtained. The method is characterized by obvious effect on removing pollutants, high product yield and low product degrading speed; and the lutein ester is further made into an oil soluble substance which has stronger stability, thereby solving the problem that the lutein ester product is easily oxidized and not easy for storing, etc.

Description

technical field [0001] The invention belongs to the technical field of phytochemistry, and in particular relates to a method for separating and purifying high-content lutein esters from marigold flower grains. Background technique [0002] US4,048,203 dissolves marigold oleoresin in hot alkanols containing no more than 4 carbon atoms, precipitates lutein esters by cooling the solution, removes alkanols by filtration, and then vacuum-dries, but the lutein esters obtained by this method The concentrate content is only 51%, which does not meet the high content requirement. [0003] US6,191,293 fully extracts the marigold corolla (or flower) with a hydrocarbon solvent to remove plant residues, evaporates the extract to obtain marigold oleoresin, and obtains an extract by alcohol precipitation at room temperature. The purity of lutein ester in the oleoresin obtained by this method varies greatly due to the quality of raw materials. [0004] CN1,432,567A extracts marigold oleore...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C403/24A61K36/28
Inventor 吴文忠黄媛徐维锋刘强冯波
Owner INNOBIO CORP LTD
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