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Preparation method of fucoxanthin

A fucoxanthin and xanthin technology, applied in the direction of organic chemistry, can solve the problem of low purity, failure to obtain high-purity fucoxanthin, failure to obtain fucoxanthin and high-value development of fucoxanthin series products Application and other issues

Active Publication Date: 2013-04-03
THIRD INST OF OCEANOGRAPHY STATE OCEANIC ADMINISTATION
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] At present, there are some research reports about fucoxanthin extraction methods: as Chinese patent CN1706836A discloses a method for isolating fucoxanthin from seaweed, the method uses repeated silica gel column chromatography separation, and uses dimethyl Alum, which cannot be removed by low-temperature vacuum distillation, makes it difficult to dry samples at low temperature and obtain high-purity fucoxanthin
Chinese patent CN100999508A discloses a method for extracting fucoxanthin from brown algae, which only uses macroporous adsorption column chromatography to separate, and the obtained sample content is 1-20%, and the purity is low
Chinese patent CN102336725 discloses a method for extracting a concentrate containing fucoxanthin from seaweed, the method uses enzyme treatment, the extract concentrate is not separated, and the purity is low
In summary, none of the above preparation methods can obtain high-purity fucoxanthin, and cannot carry out high-value development and application of fucoxanthin and fucoxanthin series products. Therefore, it is necessary to invent a Extract and separate high-purity fucoxanthin from algae or other algae for high-value development and application of fucoxanthin

Method used

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  • Preparation method of fucoxanthin
  • Preparation method of fucoxanthin
  • Preparation method of fucoxanthin

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Embodiment 1

[0030] (1) Extraction of raw materials: Take 1 kg of kelp, wash it, dry it in a cool place, add 5 L of methanol, extract it ultrasonically for 30 minutes, filter, extract twice in the same way, combine the extracts, concentrate under reduced pressure, and obtain fucoxanthin extract paste;

[0031] (2) Preliminary separation and purification: use macroporous adsorption resin for column chromatography, elute with aqueous solution, 30% ethanol aqueous solution, 60% ethanol aqueous solution, and 90% ethanol aqueous solution, collect the eluted part of 90% ethanol aqueous solution, concentrate and dry , obtain 260 mg of crude product of fucoxanthin, content 25%;

[0032] (3) Fucoxanthin refining:

[0033] a) Preparation of raw materials: the crude product of fucoxanthin is prepared into a 5 mg / ml solution;

[0034] b) Instrument: semi-preparative high performance liquid chromatography;

[0035] c) Chromatographic conditions: the semi-preparative chromatographic column is a C8 co...

Embodiment 2

[0039] 1) Extraction of raw materials: Take 1 kg of kelp, wash it, dry it in a cool place, add 5 L of ethanol, extract it ultrasonically for 60 minutes, filter, extract twice in the same way, combine the extracts, concentrate under reduced pressure, and obtain fucoxanthin extract ;

[0040] 2) Preliminary separation and purification: use macroporous adsorption resin for column chromatography, elute with aqueous solution, 30% ethanol aqueous solution, 60% ethanol aqueous solution, 80% ethanol aqueous solution, 100% ethanol aqueous solution, collect 100% ethanol aqueous solution for elution part, concentrated and dried to obtain 150 mg of crude fucoxanthin, with a content of 53%;

[0041] 3) Refined fucoxanthin:

[0042] a) Preparation of raw materials: prepare the crude product of fucoxanthin into a 5 mg / mL solution;

[0043] b) Instrument: semi-preparative high performance liquid chromatography;

[0044] c) Chromatographic conditions: the semi-preparative chromatographic co...

Embodiment 3

[0048] 1) Extraction of raw materials: Take 1 kg of kelp, wash it, dry it in a cool place, add 5 L of acetone, extract it ultrasonically for 30 minutes, filter, extract twice in the same way, combine the extracts, concentrate under reduced pressure, and obtain fucoxanthin extract ;

[0049] 2) Preliminary separation and purification: use silica gel column chromatography, elute with dichloromethane-methanol (50:1, 25:1, 10:1, 5:1) respectively, collect (25:1 and 10:1) The eluted part was concentrated and dried to obtain 105 mg of crude fucoxanthin with a content of 87%;

[0050] 3) Refined fucoxanthin:

[0051] a) Preparation of raw materials: prepare the crude product of fucoxanthin into a 5 mg / mL solution;

[0052] b) Instrument: semi-preparative high performance liquid chromatography;

[0053] c) Chromatographic conditions: the semi-preparative chromatographic column is a C8 column (250mm×10mm), the mobile phase system is 95% methanol aqueous solution, the flow rate of th...

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Abstract

The invention discloses a preparation method of fucoxanthin and relates to the fucoxanthin. The preparation method of the fucoxanthin comprises the steps that a cleaned brown algae material is aired, and soaked by an organic solvent for extraction; an obtained extracting solution is condensed, and a fucoxanthin crude extract is obtained; the fucoxanthin crude extract is subjected to column chromatography separation; a fraction of the fucoxanthin is collected and condensed, and a fucoxanthin raw material is obtained; the obtained fucoxanthin raw material is dissolved by the organic solvent and transferred to a sample introduction bottle of a semipreparative / preparative HPLC (high performance liquid chromatograph); the semipreparative / preparative HPLC is started for separation and purification; fucoxanthin purification liquid is collected automatically through ultraviolet on-line detection or by a fraction collector triggered by a mass spectrum signal; and after the collected fucoxanthin purification liquid is decompressed, condensed, frozen and dried, the high-purity fucoxanthin is obtained. Through testing, the purity of the prepared fucoxanthin is greater than 99%.

Description

technical field [0001] The invention relates to fucoxanthin, in particular to a method for preparing high-purity fucoxanthin with a purity greater than 99%. Background technique [0002] Fucoxanthin, also known as fucoxanthin, is a natural carotenoid extracted from edible brown algae, such as Undaria pinnatifida and Laminaria japonica Aresch. The two ends of the all-trans long chain have a chemically active 5,6-epoxy unsaturated allene bond structure, which is different from other carotenoid molecules and has strong biological activity. In recent years, its multiple biological activities have been confirmed, and some potential activities are being actively explored by scientists, and it has become one of the main hot spots in the research and development of marine drugs. [0003] Fucoxanthin has various biological activities such as anti-tumor, anti-inflammation, anti-oxidation, and weight loss. First of all, in terms of anti-tumor, Okuzumi et al first reported in 1990 tha...

Claims

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Application Information

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IPC IPC(8): C07D303/32C07D301/32
Inventor 张怡评易瑞灶洪专谢全灵方华孙继鹏
Owner THIRD INST OF OCEANOGRAPHY STATE OCEANIC ADMINISTATION
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