Preparation method of fucoxanthol

A technology of fucoxanthin and fucoxanthin is applied in the field of preparation of high-purity fucoxanthin, and can solve the problems of high-value development and application of fucoxanthin series products that cannot be fucoxanthin.

Inactive Publication Date: 2015-07-22
THIRD INST OF OCEANOGRAPHY STATE OCEANIC ADMINISTATION
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, only a few domestic manufacturers extract and prepare low-content fucoxanthin raw materials (HPLC method, content <1%), which are exported to Europe, America, Japan and othe

Method used

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  • Preparation method of fucoxanthol
  • Preparation method of fucoxanthol
  • Preparation method of fucoxanthol

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] 1) Enzymolysis reaction: Take 50 mg of fucoxanthin (purity: 99%), add 50 mg of lipase, 50 mg of sodium taurocholate, dissolve in 0.1M PBS buffer solution with pH=3, and react at 20°C for 1 hour Afterwards, concentrate to dryness, add 50mL of methanol for ultrasonic extraction, filter, and concentrate the filtrate to dryness to obtain 55 mg of fucoxanthol reactant, and the conversion rate of fucoxanthol is 23%;

[0035] 2) Fucoxanthol refining:

[0036] a) Configuration of raw materials: the crude product of fucoxanthin is configured into a 6 mg / mL solution;

[0037] b) Instrument: semi-preparative high performance liquid chromatography;

[0038] c) Chromatographic conditions: the semi-preparative chromatographic column is a C8 column (250mm×10mm), and the mobile phase system is

[0039] 70% methanol aqueous solution, the mobile phase flow rate is 5mL / min, and the detection wavelength is 450nm;

[0040] d) Injection volume: 100 μL;

[0041] 100 mL of fucoxanthol prep...

Embodiment 2

[0042] 1) Enzymolysis reaction: take 50 mg of fucoxanthin (purity: 99%), add 150 mg of lipase, 100 mg of sodium taurocholate, dissolve in 0.1M PBS buffer solution with pH=7, and react at 37°C for 1 hour Afterwards, concentrate to dryness, add 50 mL of methanol for ultrasonic extraction, filter, and concentrate the filtrate to dryness to obtain 85 mg of fucoxanthol reactant, and the conversion rate of fucoxanthol is 88%;

[0043] 2) Fucoxanthol refining:

[0044] a) Configuration of raw materials: the crude product of fucoxanthol is configured into a 6 mg / mL solution;

[0045] b) Instrument: semi-preparative high performance liquid chromatography;

[0046]c) Chromatographic conditions: the semi-preparative chromatographic column is a C8 column (250mm×10mm), the mobile phase system is 80% aqueous methanol, the flow rate of the mobile phase is 6mL / min, and the detection wavelength is 450nm;

[0047] d) Injection volume: 300 μL;

[0048] 150 mL of fucoxanthol preparation soluti...

Embodiment 3

[0050] 1) Enzymolysis reaction: Take 50 mg of fucoxanthin (purity: 99%), add 500 mg of lipase, 500 mg of sodium taurocholate, dissolve in 0.1M PBS buffer solution with pH=11, and react at 70°C for 0.5 After h, concentrate to dryness, add 50mL of methanol for ultrasonic extraction, filter, and concentrate the filtrate to dryness to obtain 88mg of fucoxanthol reactant, the conversion rate of fucoxanthol is 55%;

[0051] 2) Fucoxanthol refining:

[0052] a) Configuration of raw materials: the crude product of fucoxanthol is configured into a 6 mg / mL solution;

[0053] b) Instrument: semi-preparative high performance liquid chromatography;

[0054] c) Chromatographic conditions: the semi-preparative chromatographic column is a C18 column (250mm×10mm), the mobile phase system is 90% methanol water-soluble, the flow rate of the mobile phase is 6mL / min, and the detection wavelength is 450nm;

[0055] d) Injection volume: 300 μL;

[0056] 70 mL of fucoxanthol preparation solution w...

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Abstract

The invention relates to a preparation method of fucoxanthol. The preparation method comprises the following steps: under the situation of adding a catalyst, enzymolyzing fucoxanthin by adopting lipase, reacting, generating fucoxanthol, concentrating and drying, extracting through methanol and concentrating to obtain a crude fucoxanthol extract; enabling the crude fucoxanthol extract to be used as a solution medium in a form of a mobile phase, configuring into preparation liquid to be separated, transferring the preparation liquid to be separated into a semi-preparative/preparative efficient liquid phase chromatography sampling bottle and starting a semi-preparative/preparative efficient liquid phase chromatography, wherein the mobile phase is selected from one of a methanol-water solution, an ethanol-water solution or an acetonitrile-water solution; balancing a chromatographic column, automatically sampling, separating and purifying the fucoxanthol, triggering a fraction collector through ultraviolet on-line detection and in combination with mass spectrometry detection signals, automatically collecting fucoxanthol purification liquid, and decompressing, condensing, freezing and drying the purification liquid to obtain the fucoxanthol of which the purity is larger than 99 percent. The preparation method is simple in operation, high in yield, suitable for automatic control and preparation of the high-purity fucoxanthol.

Description

technical field [0001] The invention relates to a preparation method of high-purity fucoxanthol, which belongs to the fields of food processing technology and functional health care. 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] Fucoxanthol is a metabolite of fucoxanthin that removes an acetyl group. Its structure is similar to that of fucoxanthin. It has strong biological activities, including an...

Claims

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Application Information

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IPC IPC(8): C12P17/02C07D301/32C07D303/32
Inventor 张怡评洪专易瑞灶方华谢全灵孙继鹏
Owner THIRD INST OF OCEANOGRAPHY STATE OCEANIC ADMINISTATION
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