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Method for preparing astaxanthin monoester rich in astaxanthin odd-numbered fatty acid monoester

A technology of astaxanthin and fatty acid, applied in the field of preparing astaxanthin monoester rich in odd number fatty acid monoester of astaxanthin

Inactive Publication Date: 2014-06-18
SHANDONG NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Currently there is no effective method for separating odd-numbered fatty acid monoesters (astaxanthin tridecenoate monoester and astaxanthin pentadecenoate monoester) from astaxanthin monoester

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] Example 1 Separation of Astaxanthin Odd Number Fatty Acid Monoesters (Astaxanthin Tridecenoic Acid Monoester and Astaxanthin Pentadecanoic Acid Monoester) from Astaxanthin Monoesters

[0018] Proceed as follows:

[0019] (1) Preparation of Antarctic krill shrimp oil: take Antarctic krill, ventilate and dry to constant weight at 35°C-65°C, crush to 20 mesh, extract 3 times with No. 6 gasoline at 30°C, 1 hour each time, oil The liquid ratio is 1:6 (mass ratio) to obtain crude oil, and then extract the crude oil with acetone at 30°C for 3 times, each time for 0.5h, and the material-to-liquid ratio is 1:5 (mass ratio) to remove insoluble The residue of Antarctic krill shrimp oil;

[0020] (2) Extraction of astaxanthin monoester: 68g 200-300 mesh GF 254 Silica gel was activated in a drying oven at 120°C for 12 hours, then dissolved in petroleum ether and packed into a column for later use; according to the volume ratio, petroleum ether:ethyl acetate=10:1, 9:1, 8:1, 7:1, 6 ...

Embodiment 2

[0026] Example 2 Separation of Astaxanthin Odd Number Fatty Acid Monoesters (Astaxanthin Tridecenoic Acid Monoester and Astaxanthin Pentadecanoic Acid Monoester) from Astaxanthin Monoesters

[0027]Proceed as follows:

[0028] (1) Preparation of Antarctic krill shrimp oil: take Antarctic krill, ventilate and dry to constant weight at 35°C-65°C, crush to 20 mesh, extract 3 times with No. 6 gasoline at 30°C, 1 hour each time, oil The liquid ratio is 1:6 (mass ratio) to obtain crude oil, and then extract the crude oil with acetone at 30°C for 3 times, each time for 0.5h, and the material-to-liquid ratio is 1:5 (mass ratio) to remove insoluble The residue of Antarctic krill shrimp oil;

[0029] (2) Extraction of astaxanthin monoester: 68g 200-300 mesh GF 254 Silica gel was activated in a drying oven at 120°C for 12 hours, then dissolved in petroleum ether and packed into a column for later use; according to the volume ratio, petroleum ether:ethyl acetate=10:1, 9:1, 8:1, 7:1, 6 ...

Embodiment 3

[0035] Example 3 Separation of Astaxanthin Odd Number Fatty Acid Monoesters (Astaxanthin Tridecenoic Acid Monoester and Astaxanthin Pentadecanoic Acid Monoester) from Astaxanthin Monoesters

[0036] Proceed as follows:

[0037] (1) Preparation of Antarctic krill shrimp oil;

[0038] (2) Extraction of astaxanthin monoester;

[0039] The first two steps prepare astaxanthin monoester according to the method of Example 1 in the patent application whose publication number is CN102746205A;

[0040] (3) Preparation of AgNO 3 High-efficiency thin-layer plate: take a 10cm×20cm thin-layer chromatography silica gel plate H, put it on a plate with a mass concentration of 2.5% AgNO 3 Soak it in methanol solution for 4 minutes, take it out and dry it in the air for 2.5 hours, then put it in a drying oven at 45°C and dry it for 1 hour, that is, it is ready for use.

[0041] (4) Take out 20mg of the prepared Antarctic krill astaxanthin monoester from the refrigerator (-26°C), dissolve it ...

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PUM

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Abstract

The invention discloses a method for preparing astaxanthin monoester rich in astaxanthin odd-numbered fatty acid monoester. The method comprises the following steps: dissolving the astaxanthin monoester in dichloromethane, dropwise adding the mixture so as to form a line on an AgNO3 high-efficiency thin layer plate by using a capillary sample application tube, then putting on a glass chromatographic jar with a developing agent, and developing; after developing, taking out, airing, scraping off two strips, carrying out ultrasound treatment, centrifuging, taking a liquid supernatant, repeatedly extracting until the strips scrapped off are colorless, respectively obtaining extracting solutions to which the two strips respectively correspond, and carrying out rotary evaporation so as to remove the dichloromethane, thus obtaining two samples, wherein the first red strip is the astaxanthin monoester containing 7-9% of astaxanthin tridecylenic acid monoester and 48-51% of astaxanthin pentadecanoic acid monoester. The method has the advantages that the astaxanthin monoester rich in the odd-numbered fatty acid is obtained by using a AgNO3 high-efficiency thin layer plate separation method, the separation of the astaxanthin monoester is pushed forward greatly, and the method provides a basis for the separation of the astaxanthin odd-numbered fatty acid and lays a foundation for the future secondary separation and purification.

Description

technical field [0001] The invention relates to a method for preparing astaxanthin monoester rich in astaxanthin odd fatty acid monoester (astaxanthin tridecenoate monoester and astaxanthin pentadecenoate monoester). Background technique [0002] Antarctic krill is a key species in the biological chain of the Southern Ocean. It is the single species of biological resource with the largest biomass energy and the most successful evolution in the world, about 600-5000 million tons (there is a big difference due to different estimation methods, and the lowest conservative estimate is also 600-1000 million tons), with an annual catch of 100-150 million tons, which is more than the world’s total annual fishery catch (99 million tons). my country has 1.8 billion mu of arable land, and its annual grain output is nearly 600 million tons. Antarctic phosphorus The annual catchable amount of shrimp is equivalent to 300-450 million mu of arable land, which is a huge overseas resource. [...

Claims

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Application Information

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IPC IPC(8): C07C403/24C11B1/10C11B7/00
Inventor 张沙沙苏树朋刘代成
Owner SHANDONG NORMAL UNIV
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