Method for preparing ergothioneine

A technology of ergothioneine and concentration, applied in the direction of organic chemistry, etc., can solve the problems of waste, low content of ergothioneine extract, difficulty in large-scale production, etc., achieve huge economic benefits, reduce production costs, reduce waste of resources and Effects of Environmental Pollution

Active Publication Date: 2017-06-13
天津华泰至成医药科技发展有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The problem with the existing natural raw material extraction method is that the content of the ergothioneine extract obtained by the existing extraction method is very low, generally only about 1% to 5%, and it is diffi

Method used

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  • Method for preparing ergothioneine
  • Method for preparing ergothioneine
  • Method for preparing ergothioneine

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] The conditions of the HPLC detection method for ergothioine:

[0031] Column: Kromasil 100-5NH 2 Column (250mm×4.60mm, E36056)

[0032] Detection wavelength: 254nm

[0033] Flow rate: 1.0ml / min

[0034] Column temperature: 30℃

[0035] Mobile phase: acetonitrile-5mmol / L ammonium acetate (80:20)

[0036] Injection volume: 20μL.

Embodiment 2

[0038] (1) Extraction: Add 500g of water to 100g of Hazel mushrooms, and extract 3 times at 95°C for 3, 2 and 1 hours of extraction time. Filter. The mesh number of the filter is 120. Combine the filtrate. Leave it to cool down until the temperature is lower than 50°C, discard the precipitate, and get the supernatant;

[0039] (2) Macroporous resin adsorption and separation: The supernatant obtained in (1) is adsorbed on HP20 type macroporous resin, water, and the volume percentage concentration is 5%, 15%, 25%, 35%, 50% ethanol aqueous solution Gradient elution, each 250ml is used as a receiving volume. Analytical HPLC is used to collect ergothioine-rich eluents, combine the eluents, and then under the condition that the temperature is ≤60℃ and the vacuum degree is 0.06~0.08MPa Concentrate under reduced pressure with a sugar content of 40 to obtain a macroporous resin separation product;

[0040] (3) Polyamide resin separation: disperse the macroporous resin separation product ob...

Embodiment 3

[0042] This embodiment includes four steps, among which steps (1) to (3) are the same as in embodiment 2, and step (4) operates as follows.

[0043] (4) ODS low-pressure column chromatography separation: the thioneine extract obtained by step (3) polyamide separation is adsorbed on ODS low-pressure column with water and the volume percentage concentration is 5%, 10%, 20%, 35 5% ethanol aqueous solution for gradient elution, each 25ml as a receiving volume, detected by analytical HPLC, with pure thioneine as the reference substance, collect the eluate rich in thioneine, and then at the temperature ≤60℃, Concentrate under reduced pressure under the condition of a vacuum degree of 0.06 to 0.08 MPa to obtain a concentrated thioneine product with a sugar content of 10. Measured by the method of Example 1, the content of ergothioneine is 80.1%.

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Abstract

The invention provides a method for preparing ergothioneine. The method takes mushrooms or leftovers as raw materials and comprises the following steps: extracting the raw materials in water or an ethanol water solution with the volume percent concentration of 5 percent to 30 percent at the temperature of 70 DEG C to 95 DEG C; sequentially separating and purifying an extracted product through macroporous resin and polyamide resin; collecting an eluting solution and concentrating to obtain ergothioneine extract. Compared with the prior art, the extract with the ergothioneine content of 20 percent to 98 percent can be obtained and the content is much higher than 1 percent to 5 percent in the prior art. The ergothioneine prepared by the invention can reach requirements of industrialized production and lays a foundation for further development and utilization of the ergothioneine extract.

Description

Technical field [0001] The present invention relates to the technical field of preparation of active ingredients, in particular to a method for preparing ergothioneine from mushrooms or their scraps. Background technique [0002] Ergothioneine (ergothioneine, abbreviated as EGT) is a rare amino acid discovered in ergot in 1909. Its molecular structure is shown below. [0003] [0004] Ergothioneine is an important active substance in the body, but it cannot be synthesized by the animal body itself and can only be ingested from food. Foreign studies have shown that it can act as an antioxidant in the organism, has various physiological functions such as scavenging free radicals, maintaining DNA biosynthesis, normal cell growth and cellular immunity. It can be used in outdoor skin care products, protective cosmetics and ophthalmology. The development of products, which can also be used as an ideal substitute for glutathione, has gradually gained more attention. Experiments have sho...

Claims

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Application Information

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IPC IPC(8): C07D233/84
CPCC07D233/84
Inventor 刘成航刘岱琳赵艳敏李长惠
Owner 天津华泰至成医药科技发展有限公司
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