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

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Example Embodiment

[0027] Example 1

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

Example Embodiment

[0029] Example 2

[0030] Weigh 100g of the ointment with 28% lutein ester content and put it into a small pressurized reactor, add 300ml solvent A (20% hexane volume fraction, 35% methyl acetate, 50% ethanol), and the purity of the inlet is 99% Make the pressure (gauge pressure) reach 0.1Mpa with nitrogen, stir for 10min at a temperature of 35℃, 450r / min, release the pressure and cool to 10℃, filter to obtain filter cake I, weight 72g; put filter cake I and 150ml solvent A into the reaction The tank is filled with nitrogen with a purity of 99% to make the pressure (gauge pressure) reach 0.5Mpa, stirred at 50°C and 450r / min for 5 minutes, cooled to 20°C, and filtered after pressure relief. The filter cake obtained repeats this process twice. Obtain filter cake II, weighing 51g; filter cake II and 65g solvent B (85% ethanol, 15% n-hexane) at room temperature, nitrogen pressure to 0.5Mpa, 450r / min, stir for 5min, filter cake III, It weighs 39g, washed twice with 50ml of 99% ethano...

Example Embodiment

[0031] Example 3

[0032] Weigh 5kg of the 31% ointment with lutein ester content and put it into a 30L magnetically stirred pressure reactor, add 12.5L solvent A (25% hexane volume fraction, 35% ethyl acetate, 40% ethanol), and pass the purity to 99% nitrogen makes the pressure (gauge pressure) reach 0.5Mpa, the temperature is 40℃, 450r / min stirring for 10min, pressure relief and cooling to 10℃, filter cake I, weight 3.8kg; put filter cake I and 5L solvent A In the reaction tank, pass nitrogen with purity of 99% to make the pressure (gauge pressure) reach 0.8Mpa, stir at 40℃, 450r / min for 10min, cool to 20℃, release the pressure and filter, and then repeat this process twice for the obtained filter cake , Get 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, stir for 5min, filter cake III, weighing 2.05kg, washed twice with 2.4L95% ethanol under normal temperature and pressure...

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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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