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Crystalline oxidized glutathione and production method therefor

A technology of oxidized glutathione and glutathione, which is applied in the preparation method of peptides, chemical instruments and methods, crystal growth, etc., can solve the problem of impurity increase and impurity elimination (poor purification ability and crystal separation ability) And other issues

Active Publication Date: 2015-07-22
KYOWA HAKKO BIO CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] However, it is known that the production method by freeze-drying an oxidized glutathione solution has poor impurity elimination and requires a large amount of energy for freeze-drying, so it is not suitable for industrialization.
At the same time, methods based on spray drying are known to increase impurities due to thermal exposure
[0005] Furthermore, it is known that crystals of oxidized glutathione octahydrate have problems in that the crystals contain non-uniform water content, are poor in stability and require a long time of up to 3-4 days to obtain crystals; and oxidized The crystal of glutathione monohydrate has room for improvement because it is poor in crystal separation ability due to its needle-like crystal and easy to agglomerate, and its impurity elimination (purification ability) is poor and its crystal growth rate is slow

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0058] Production of crystals of oxidized glutathione hexahydrate (1)

[0059] The freeze-dried powder (3.0 g) of oxidized glutathione obtained in Reference Example 1 was dissolved in water to provide an aqueous solution containing oxidized glutathione (30 mL, oxidized glutathione concentration: 100 g / L). The aqueous solution was allowed to stand at 5°C for 48 hours to precipitate crystals. The precipitated crystals were separated by filtration and dried under ventilation to obtain crystals (1.0 g) of oxidized glutathione hexahydrate. In addition, single crystal X-ray structure analysis showed that the crystal was hexahydrate.

[0060] Hereinafter, the physicochemical properties of the obtained oxidized glutathione hexahydrate will be described.

[0061] Hydration number: hexahydrate

[0062] Melting point: 191°C

[0063] Powder X-ray diffraction [diffraction angle (2θ°), the number in parentheses indicates the relative intensity ratio (I / I 0 )]: 8.12°(100), 9.70°(33), 10.62°(43), 12...

Embodiment 2

[0068] Production of crystals of oxidized glutathione hexahydrate (2)

[0069] The freeze-dried powder (10.0 g) of oxidized glutathione obtained in Reference Example 1 was dissolved in water to provide an aqueous solution containing oxidized glutathione (33 mL, oxidized glutathione concentration: 300 g / L). The aqueous solution was cooled to 5°C and the crystals (0.1 g) obtained in Example 1 were added thereto as seed crystals. Methanol (66 mL) was added to the resultant solution for 5 hours for crystallization. The crystallization solution was aged for 1 hour, and the precipitated crystals were separated by filtration and dried under ventilation to obtain crystals of oxidized glutathione hexahydrate (8.5 g).

Embodiment 3

[0071] Production of oxidized glutathione crystals (3)

[0072] An aqueous solution containing reduced glutathione was obtained according to the method described in Example 2 of Japanese Patent Laid-Open No. 61-74595, and adjusted with an aqueous sodium hydroxide solution according to the method described in Japanese Patent Laid-Open No. 5-146279 After reaching pH 7.5, oxygen was blown into the system for oxidation, thereby obtaining an aqueous solution containing oxidized glutathione (48.1 L, oxidized glutathione concentration: 18.0 g / L).

[0073] The aqueous solution was adjusted to pH 3.0 with sulfuric acid and subjected to sterilization treatment to obtain a sterilization solution of oxidized glutathione (55.5 L, oxidized glutathione concentration: 14.4 g / L). The sterilization solution was injected onto Diaion SK116 (22L), and then onto DowexXUS-40232.01 (13L) for adsorption of oxidized glutathione. Ammonia solution (20L, concentration: 2mol / L) The oxidized glutathione is elut...

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Abstract

Provided is a novel crystal of oxidized glutathione hexahydrate. Crystal of oxidized glutathione hexahydrate is produced by cooling an aqueous solution containing oxidized glutathione to 15°C or lower to precipitate a crystal of oxidized glutathione hexahydrate.

Description

Technical field [0001] The present invention relates to crystals of oxidized glutathione and a manufacturing method thereof. The crystals can be used as products, raw materials, intermediates, etc. of health food, medicine, cosmetics and the like. Background technique [0002] Oxidized glutathione and reduced glutathione have the same action, and as the action of oxidized glutathione, for example, oral detoxification of the liver is known (Non-Patent Document 1). Therefore, oxidized glutathione can be used in various applications using reduced glutathione, for example, it can be used as a product, raw material, or intermediate for health food, medicine, cosmetics, and the like. [0003] Known methods for producing oxidized glutathione include a method in which an aqueous solution or yeast extract containing reduced glutathione obtained by a fermentation method, an enzymatic method, etc., is used as a raw material, and the aqueous solution is Or in yeast extract, convert reduced gl...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07K5/037C07K1/14
CPCC30B7/08C07K5/0215C30B29/54
Inventor 木村研福元健太田中浩志
Owner KYOWA HAKKO BIO CO LTD