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Method for preparing high-content natural lutein ester rapidly

A technology of lutein ester and lutein, which is applied in the field of preparation of food-grade lutein ester, can solve the problems that the viscous components in the lutein ointment cannot be removed, the lutein ointment is difficult to disperse, and the crystal purity is difficult to improve. , to achieve the effect of easy large-scale industrial production, low solvent consumption and short time consumption

Active Publication Date: 2018-05-04
GUANGZHOU LEADER BIO TECH +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the defect of this process is that the short-chain alcohol cannot fully remove the viscous components in the lutein ointment, and the lutein ointment is not easy to disperse in the alcohol, requiring higher temperature and longer stirring time, which all bring The problem of energy consumption and loss, and the final crystal purity is difficult to improve

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Weigh 100g of ointment with a lutein ester content of 31% and put it into a small magnetic stirring pressure reactor, add 200ml of solvent A (15% n-hexane volume fraction, 40% methyl acetate, 45% methanol), and feed it with a purity of 99% % nitrogen to make the pressure reach 1Mpa, temperature 50°C, 250r / min stirring for 25min, release pressure and cool to 20°C, filter cake I, weight 80g; put filter cake I and 80ml solvent A into the reaction tank, pass into the purity Use 99% nitrogen to make the pressure reach 0.5Mpa, stir at 20°C and 250r / min for 20min, release the pressure and filter, and repeat the process 3 times for the obtained filter cake to obtain filter cake II, weighing 48g; mix filter cake II with 40ml Solvent B (75% ethanol, 25% n-hexane) was stirred for 10 minutes at room temperature, under the conditions of nitrogen flow and pressure to 0.5Mpa, 250r / min, and filtered to obtain filter cake III, weighing 42g, and then washed twice with 50ml of 95% ethanol....

Embodiment 2

[0030] Weigh 100g of ointment with a lutein ester content of 28% and put it into a small pressurized reaction tank, add 300ml of solvent A (20% n-hexane volume fraction, 35% methyl acetate, 50% ethanol), and the purity of the feed is 99%. The nitrogen gas makes the pressure (gauge pressure) reach 0.1Mpa, stir at 35°C, 450r / min for 10min, release the pressure and cool to 10°C, filter to obtain filter cake I, weighing 72g; put filter cake I and 150ml of solvent A into the reaction Tank, feed nitrogen gas with a purity of 99% to make the pressure (gauge pressure) reach 0.5Mpa, stir at 50°C and 450r / min for 5min, cool to 20°C, and filter with pressure relief, and repeat this process twice for the obtained filter cake. Filter cake II was obtained, weighing 51 g; filter cake II and 65 g of solvent B (ethanol 85%, n-hexane 15%) were stirred for 5 minutes at room temperature, under nitrogen and pressurized to 0.5 Mpa, 450 r / min, and filtered to obtain filter cake III. Weighing 39g, wa...

Embodiment 3

[0032]Weigh 5 kg of ointment with a lutein ester content of 31% and put it into a 30L magnetic stirring pressure reaction tank, add 12.5L of solvent A (25% of n-hexane volume fraction, 35% of ethyl acetate, 40% of ethanol), and feed the mixture with a purity of 99% nitrogen to make the pressure (gauge pressure) reach 0.5Mpa, temperature 40°C, stir at 450r / min for 10min, release pressure and cool to 10°C, filter cake I, weight 3.8kg; put filter cake I and 5L solvent A into Into the reaction tank, feed nitrogen with a purity of 99% to make the pressure (gauge pressure) reach 0.8Mpa, stir at 40°C and 450r / min for 10min, cool to 20°C, and filter with pressure release, and repeat the process twice for the obtained filter cake , to obtain filter cake II, weighing 2.85kg; filter cake II and 3L solvent B (ethanol 75%, n-hexane 25%) at room temperature, nitrogen pressure to 0.5Mpa, 450r / min under stirring for 5min, filter to obtain filter cake III, weighing 2.05kg, was washed twice wit...

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PUM

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Abstract

The invention relates to a method for preparing high-content natural lutein ester rapidly. Natural lutein ester crystals are prepared by using solvents with different properties to form a ternary solvent system, taking marigold ointment with the lutein ester content being 20 to 40 percent as a raw material and washing and filtering under the relative pressure of 0 to 1 Mpa. The lutein ester prepared by the method has high flowability and is loose crystals, and the crystal powder after drying is orange and bright. The process is simple, the washing efficiency is high, extremely short time is consumed, the obtained lutein ester has high purity, the used solvents can be recycled, and the method is suitable for large-scale industrial production.

Description

technical field [0001] The invention belongs to the field of separation and purification of natural products, and in particular relates to a method for preparing food-grade lutein ester from marigold ointment. Background technique [0002] Lutein has many functions such as coloring, anti-oxidation, eye protection, anti-cardiovascular disease and anti-cancer, etc. It is widely used in food, medicine, eye health products, cosmetics and aquaculture and other fields. Lutein fatty acid ester is the form of lutein in plants. The human body cannot synthesize lutein by itself and must be supplemented through diet. Lutein esters in fruits and vegetables enter the human body through diet and are hydrolyzed into lutein monomers, which are absorbed and utilized by the human body. Lutein in nature is mainly in the all-trans configuration. In plants such as marigolds, the content of lutein in a free state is relatively small, and most of it is combined with long-chain saturated fatty ac...

Claims

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Application Information

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IPC IPC(8): C07C403/24
CPCC07B2200/13C07C403/24
Inventor 姚翰林劲冬许雪磊陶正国
Owner GUANGZHOU LEADER BIO TECH
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