Method for preparing high-content xanthophyll crystal from Calendula officinalis extract
A technology for lutein and extract, applied in the field of preparing high-content lutein crystals, can solve the problems of high cost, difficult separation, large amount of organic solvent, etc., and achieves reduced preparation cost, less damage and loss, and less environmental pollution Effect
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Embodiment 1
[0030] Weigh 40g of Calendula officinalis extract (content is 150g / kg) in a 100ml round-bottomed flask, add 5g of sodium hydroxide and 10g of methanol successively under electromagnetic stirring, add 0.2g of vitamin C, bathe in 60°C water, fill with nitrogen protection, and react for 2.5 hour, add 20 parts of 5°C deionized water to dilute, centrifuge, collect the filter residue, wash the filter residue with 5°C deionized water until the pH value of the effluent liquid is 6.5, and vacuum dry to obtain crude lutein. The crude lutein was washed twice with 10 parts of n-hexane each, and centrifuged, and the lutein crystals were dissolved in methylene chloride at room temperature to obtain a saturated solution, and 0.2 times of n-hexane was added dropwise to the saturated solution until turbidity appeared , centrifuged. The freeze-drying time is 20 hours. Obtain 5.6g of 98% lutein crystals. The effective conversion rate was 91.5%.
Embodiment 2
[0032] Weigh 250g of Calendula officinalis extract (content is 150g / kg) in a 500ml round-bottomed flask, add 16g of potassium hydroxide and 34g of methanol in turn under electromagnetic stirring, add 1.2g of vitamin E, put in a water bath at 60°C, fill with nitrogen protection, and react for 2.5 Add 20 parts of 5°C deionized water for dilution, centrifuge, collect the filter residue, wash the filter residue with 5°C deionized water until the pH value of the effluent liquid is 6.7, and vacuum dry to obtain crude lutein. Wash the crude lutein twice with 10 parts of n-hexane, centrifuge, dissolve the lutein crystals in dichloromethane at room temperature to obtain a saturated solution, add 0.3 times of n-hexane dropwise to the saturated solution until it becomes turbid , centrifuged. The freeze-drying time is 20 hours. 35.5 g of 97.7% lutein crystals were obtained. The effective conversion rate was 92.5%.
Embodiment 3
[0034] Weigh 100g of Calendula officinalis extract (content is 150g / kg) into a 250ml round-bottomed flask, under electromagnetic stirring, potassium hydroxide 6g, ethanol 22g, vitamin E 0.5g, 60 ℃ water bath, nitrogen protection, reaction 2.5 Add 20 parts of 5°C deionized water for dilution, centrifuge, collect the filter residue, wash the filter residue with 5°C deionized water until the pH value of the effluent liquid is 7.0, and vacuum dry to obtain crude lutein. Wash the crude lutein twice with 8 parts of n-hexane, centrifuge, dissolve the lutein crystals in dichloromethane at room temperature to obtain a saturated solution, add 0.3 times of n-hexane dropwise to the saturated solution until it becomes turbid , centrifuged. The freeze-drying time is 20 hours. 14.3 g of 97.5% lutein crystals were obtained. The effective conversion rate was 93.0%.
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