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Method for separating and purifying all-trans high-purity lutein esters powder

A technology for separation and purification of lutein esters, applied in the field of phytochemistry, can solve the problems of increased difficulty in manufacturing ultrasonic equipment, high requirements for supercritical extraction equipment, and unacceptable costs for users, so as to reduce labor costs and power costs, The effect of easy regeneration and easy operation

Active Publication Date: 2012-12-26
NORTH CHINA PHARMA HEBEI HUANUO
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This extraction method has certain defects: supercritical extraction requires high equipment, small processing capacity, and high production cost
This method has the following disadvantages: (1) Restricted by ultrasonic attenuation factors, the effective area of ​​ultrasonic action is a ring. If the diameter of the extraction tank is too large, an ultrasonic blank area will be formed on the peripheral wall of the tank; (2) It is difficult to match the power of the tank The volume of the tank (generally 3000 liters to 6000 liters) is matched, and the 6000 liter tank needs 120 to 180kw ultrasonic output power. Such a large power makes it more difficult to manufacture ultrasonic equipment, and at the same time, the cost cannot be accepted by users.

Method used

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  • Method for separating and purifying all-trans high-purity lutein esters powder

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0042] At 20°C, take 50kg marigold pellets (the total content of total carotenoid-lutein diester, zeaxanthin ester and other carotenoids and their fatty acid esters is 4.0%). Feed the material at the feed inlet of the head of the extraction tube, add 50L n-hexane from the solvent inlet at the end of the continuous countercurrent ultrasonic extraction tube, and perform continuous countercurrent ultrasonic extraction. Granules to obtain 52L lutein ester extract. The extract was concentrated in vacuo at 30°C to obtain 4.0L crude extract of lutein ester. The crude extract was chromatographed through a resin column with a height-to-diameter ratio of 5:1 and a capacity of 12 L of acidic alumina. The saturated resin was desorbed with ethyl acetate at a desorption flow rate of 6 L / h to obtain 40 L of analytical solution. The stripped solution was concentrated in vacuo at 30° C. to obtain 2.2 L of lutein ester concentrate. Then slowly add 6.6L of isopropanol, slowly lower the temper...

Embodiment 2

[0044] At 30°C, take 100kg marigold granules (the total content of carotenoids-lutein diester, zeaxanthin ester and other carotenoids and their fatty acid esters is 4.2%). Feed the material at the feed port at the head of the extraction tube, add 500L cyclohexane from the solvent inlet at the end of the continuous countercurrent ultrasonic extraction tube, and perform continuous countercurrent ultrasonic extraction with an ultrasonic frequency of 40-50 KHz, continuous countercurrent ultrasonic extraction for 2-3 hours, Frame press filtration, wash the marigold granules, and obtain 510L lutein ester extract. The extract was concentrated in vacuo at 40°C to obtain 17.1L crude extract of lutein ester. The crude extract was chromatographed through a resin column with a height-to-diameter ratio of 6:1-8:1 and a neutral alumina loading capacity of 68L. The saturated resin was desorbed with ethyl acetate at a desorption flow rate of 100 L / h to obtain 270 L of analytical solution. T...

Embodiment 3

[0046] At 55°C, 100kg of marigold granules (containing total carotenoid-lutein diester, zeaxanthin ester, and other carotenoids and their fatty acid esters totaling 2.2%) were subjected to continuous countercurrent ultrasonic Feed the material at the feed inlet at the head of the extraction tube, add 1000L isopropyl ether from the solvent inlet at the end of the continuous countercurrent ultrasonic extraction tube, and perform continuous countercurrent ultrasonic extraction with an ultrasonic frequency of 80 KHz, continuous countercurrent ultrasonic extraction for 1 hour, membrane filtration and washing Chrysanthemum granules to obtain 1100L lutein ester extract. The extract was concentrated in vacuo at 50°C to obtain 20.2L crude extract of lutein ester. The crude extract was chromatographed through a resin column with a height-to-diameter ratio of 10:1 and a basic alumina loading capacity of 100 L. The saturated resin was desorbed with ethyl acetate at a desorption flow rate...

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Abstract

The invention discloses a method for separating and purifying all-trans lutein esters powder prepared by Tagetes erecta granules, comprising the steps of mixing the Tagetes erecta granules and nonpolar solvent to perform continuously countercurrent supersonic extraction to obtain extract liquid, concentrating the extract liquid to obtain crude extract liquid extracts, dissolving the crude extract liquid extracts by solvent and using alumina column to perform column chromatography to obtain the high-purity lutein esters products. According to the invention, the continuously countercurrent supersonic extraction is adopted to extract lutein esters, and the method has large batch processing capacity, less solvent using amount and high recovery rate, can reduce labor and power expenses, solves the technical problem that the lutein esters are directly purified from crude Tagetes erecta extracts by adopting the alumina column to perform chromatography of the lutein esters, and can prepare the all-trans lutein esters products with content more than 95% (HPLC: High Performance Liquid Chromatography), wherein the total carotenoid yield is more than 80 percent.

Description

technical field [0001] The invention belongs to the technical field of phytochemistry, and in particular relates to a method for separating and purifying high-content lutein esters from marigold granules. Background technique [0002] Lutein ester is the ester formed by lutein and long-chain unsaturated fatty acid. It is the main form of lutein in plants and widely distributed in nature. The content of lutein ester in marigold (Tagetes erecta L) The most abundant, as high as 30% to 40%, it is an important industrial source of lutein esters. Lutein esters are a mixture of various esters, including monoesters, diesters and mixed diesters, among which dipalmitate contains the most, and its structural formula is as follows: [0003] [0004] R1 R2 Lutein H H lauric monomyristate Lauric acid myristic acid Dimyristate myristic acid myristic acid myristyl palmitate myristic acid palmitic acid dipalmitate Palmitic acid Palmi...

Claims

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Application Information

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IPC IPC(8): C07C403/24
Inventor 张雪霞可爱兵李宁李晓露任风芝陈书红王海燕成晓迅林毅李丽红张金娟林旸张丽张艳立高月麒张艳哲蒋沁孟雅娟朱秀良段宝玲
Owner NORTH CHINA PHARMA HEBEI HUANUO
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