A kind of method for preparing high stability canthaxanthin in high yield
A high-stability, canthaxanthin technology, applied in the field of nutritional chemicals, can solve the problems of poor storage stability of canthaxanthin crystals, difficult to apply to industrialization, unstable hypobromous acid, etc., so as to improve the oxidation reaction yield and storage. The effect of improving stability and improving yield
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[0033] The preparation process of β-carotene can refer to patent CN110452147A. In this process, TPPO will inevitably enter into β-carotene crystals, thereby affecting the subsequent oxidation reaction, and finally entering canthaxanthin. The content of TPPO in the β-carotene prepared by the patented method is generally as high as 5000-10000 ppm.
[0034] In the present invention, the content of TPPO in β-carotene can be effectively controlled by washing with dichloromethane and ethanol mixed solvents in different amounts and proportions. In the mixed solvent, the mass ratio of dichloromethane and ethanol is 1:0.5-2, and the washing time is 3-6h.
[0035] Specifically, when the dosage of the mixed solvent is 10-20 times the dosage of β-carotene, the TPPO content can be reduced to below 1000ppm; when the dosage of the mixed solvent is 20-50 times the dosage of β-carotene, the TPPO content can be reduced to 500ppm or less; when the amount of mixed solvent is 50-100 times that of...
preparation example
[0051] The β-carotene with high content of TPPO is prepared with reference to the method in Example 2 of Patent CN110452147A, and the TPPO content of the obtained β-carotene is about 6000 ppm. Use a mixed solvent of dichloromethane and ethanol to wash the beta-carotene, the mass ratio of dichloromethane and ethanol in the mixed solvent is 1:1, and the amount of the mixed solvent is controlled to be 10-100 times the amount of beta-carotene, and the washing The time is 3-6h, and β-carotene with different contents of TPPO is obtained.
[0052] When the mixed solvent dosage is 28 times and the washing time is 4h, the TPPO content is reduced to 450ppm;
[0053] When the mixed solvent dosage is 55 times and the washing time is 6h, the TPPO content is reduced to 180ppm;
[0054] When the amount of mixed solvent is 18 times and the washing time is 3h, the TPPO content is reduced to 980ppm;
[0055] When the mixed solvent dosage is 95 times and the washing time is 6h, the TPPO conten...
Embodiment 1
[0060] Mix β-carotene (TPPO content is 450ppm), sodium hypochlorite, sodium iodide, water, and dichloroethane in a mass ratio of 1:0.08:1:20:60, and react at 20°C and 0.3MPaA for 10 hours. After quenching, washing and desolventizing with sodium thiosulfate, the obtained crude canthaxanthin was mixed with ethyl acetate at a mass ratio of 1:10, reacted at 100°C and 0.5MPaA for 8 hours, and then centrifuged, washed and dried. , to obtain canthaxanthin crystals. The yield of the oxidation reaction was 83%, and the yield of the isomerization reaction was 95%. The obtained crystals were stored in nitrogen atmosphere for 30 days, and the crystal purity decreased from 99.5% to 99.2%.
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