Method for preparing food-grade lutein crystal from marigold extract
A marigold and lutein technology, applied in the direction of organic chemistry, can solve the problems of low product yield, complicated steps, and long time consumption, and achieve the effects of reducing production costs, convenient operation, and cost reduction
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Embodiment 1
[0044] 20.0g marigold extract, in which the lutein content is 156.29mg / g, add 95% ethanol whose volume is 3 times the mass of the extract, stir evenly, then add 20% of the mass of the extract as solid sodium hydroxide, at 50°C React for 6 hours until the saponification reaction is complete, add 100mL of tap water to dilute and cool down to 35°C, crystallize under slow stirring for 16 hours, adjust the pH value to 8-9 with glacial acetic acid and filter to obtain filter cake I; add 100mL of 50% ethanol to filter cake I The aqueous solution was washed at 50°C and then filtered to obtain filter cake II; the filter cake II was washed with 60 mL of 95% ethanol and then filtered, and the filter cake was dried at 60°C after adding antioxidants to obtain 3.50 g of lutein crystal powder, of which The UV content of lutein is 83.27%. According to HPLC detection, the content of all-trans lutein is 92.45%, and the pure yield of lutein is 86.20%.
Embodiment 2
[0046] 20.0g marigold extract, wherein the lutein content is 156.29mg / g, add 88% isopropanol whose volume is 5.5 times of the mass of the extract, stir well, then add 30% of the mass of the extract as solid sodium hydroxide, 50 React at ℃ for 3 hours until the saponification reaction is complete, add 105mL of tap water to dilute and cool to 45℃, crystallize under slow stirring for 24 hours, adjust the pH value to 8-9 with glacial acetic acid and filter to obtain filter cake I; add 80mL60 % isopropanol aqueous solution was washed at 50°C and then filtered to obtain filter cake II; the filter cake II was washed with 40 mL of 95% ethanol and then filtered, and the filter cake was dried at 80°C after adding antioxidants. 3.65 g of lutein crystal powder was obtained, of which the UV content of lutein was 81.52%, and the content of all-trans lutein was 91.32% through HPLC detection, and the pure yield of lutein was 86.93%.
Embodiment 3
[0048] 20.0g of marigold extract, in which the lutein content is 153.55mg / g, add 95% ethanol whose volume is 7 times the mass of the extract, stir evenly, then add 35% of the mass of the extract as solid sodium hydroxide, at 50°C React for 5 hours until the saponification reaction is complete, add 170mL of tap water to dilute and lower the temperature to 40°C, crystallize under slow stirring for 24 hours, adjust the pH value to 8-9 with glacial acetic acid and filter to obtain filter cake I; add 100mL of 60% ethanol to filter cake I The aqueous solution was washed at 60°C and then filtered to obtain filter cake II; the filter cake II was washed with 120 mL of 95% ethanol and then filtered, and the filter cake was dried at 50°C after adding antioxidants. 3.13 g of lutein crystal powder was obtained, of which the UV content of lutein was 90.20%, and the content of all-trans lutein was 92.75% through HPLC detection, and the pure yield of lutein was 85.27%.
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