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Crystallization method for sucrose trichloride

A technology of sucralose and acetyl sucralose, applied in chemical instruments and methods, sugar derivatives, sugar derivatives, etc., can solve the problems of decreased content, poor thermal stability of sucralose crystals, etc., and achieves improved stability. Effect

Inactive Publication Date: 2008-01-16
DAFENG HEGNO PHARMA +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Generally speaking, sucralose has good thermal stability during food processing, and its aqueous solution also has good thermal stability, mainly due to the low concentration of sucralose or its aqueous solution during food processing, but drying The thermal stability of the sucralose crystals is relatively poor, and the sucralose crystals quickly turn brown to brown at 100°C, and the content also decreases quickly (EP267809)

Method used

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  • Crystallization method for sucrose trichloride
  • Crystallization method for sucrose trichloride

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] In a 1000ml three-neck flask, under nitrogen protection, add 100.0g of 2,3,6,3',4'-pentaacetylsucralose with a content of 99.1%, 400.0ml of methanol, and 5.0g of 10% sodium hydroxide in methanol , After reacting at 40-45°C for 1.5-2.0 hours, the cation exchange resin was neutralized to about pH=7.0, the resin was removed by filtration, 5.0 g of activated carbon was added for decolorization, and concentrated to dryness under reduced pressure. Add 400ml of water, concentrate under reduced pressure and distill off residual methanol. Wash once with 50 ml of ethyl acetate, and concentrate the water layer under reduced pressure until the moisture reaches 25.0-30.0%. Stop the concentration, add ethanol to make the ethanol content of the crystallization solution about 5%, heat up to 75°C, cool to 40°C and stir for crystallization for 4 hours, then cool to 30°C and filter. Vacuum dried at 40°C. 42.1 g of sucralose were obtained. HPLC test content reached 98.8%.

Embodiment 2

[0024] In a 1000ml three-neck flask, under nitrogen protection, add 100.0g of 6-acetyl sucralose with a content of 98.5%, 400.0ml of methanol, add 6.0g of sodium hydroxide methanol (10%) solution, and react at 40-45°C for 1.5- After 2.0 hours, the cation exchange resin AMBERLITE IRC86 was neutralized to about pH=7.0, the resin was removed by filtration, 5.0 g of activated carbon was added for decolorization, and concentrated to dryness under reduced pressure. Add 500ml of water, concentrate under reduced pressure and evaporate residual methanol. Wash once with 50 ml of ethyl acetate, and concentrate the water layer under reduced pressure until the moisture reaches 25.0-30.0%. Add ethanol to make the ethanol content of the crystallization solution about 5%, heat up to 75°C, cool to 40°C and stir for crystallization for 4 hours, then cool to 30°C and filter. Vacuum dried at 40°C. 59.5 g of sucralose were obtained. HPLC test content reached 98.9%.

Embodiment 3

[0026] In a 1000ml three-necked flask, under nitrogen protection, add 100.0g of pentaacetylsucralose with a content of 98.5%, 400.0ml of methanol, add 6.0g of sodium hydroxide methanol solution (10%), and react at 40-45°C for 1.5-2.0 Hours later, the cation exchange resin AMBERLITE IRC86 was neutralized to about pH=7.0, the resin was removed by filtration, 5.0 g of activated carbon was added for decolorization, and concentrated to dryness under reduced pressure. Add 400ml of water, concentrate under reduced pressure and distill off residual methanol. Wash once with 50 ml of ethyl acetate, and concentrate the water layer under reduced pressure until the moisture reaches 25.0-30.0%. Stop the concentration, raise the temperature to 75°C, the system dissolves, then cool to 40°C and stir for crystallization for 4 hours, then cool to 30°C, and filter. Vacuum dried at 40°C. 43.1 g of sucralose were obtained. HPLC test content reached 98.7%.

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Abstract

The invention discloses a sucralose crystallization method. The sucralose can be crystallized in the mixed solvent of water and alcohol or the mixed solvent of water and ethyl acetate. The stability of the sucralose during storage can be improved obviously with the crystallization method.

Description

technical field [0001] The invention relates to the field of food technology. Specifically, the invention relates to a crystallization method of food sweetener-sucralose. Background technique [0002] Sucralose (Sucralose, molecular formula C12H1908Cl13, molecular weight 397.64) (I) is a new type of high-sweet non-nutritive sweetener, its chemical name is 4,1',6'-trichloro-4,1',6 '-Trideoxygalactosucrose 4,1',6'-trichlorogalactosucrose1,6-dichloro-1,6-dideoxy-β-D-fructofurannosyl-4-chloro-4-deoxy-α-D-galactopyranoside, [0003] The chemical structural formula is: [0004] [0005] The sweetness of sucralose is about 600 times that of sucrose. It does not participate in metabolism in the human body, is not absorbed by the human body, and has 0 calories. It is an ideal sweet substitute for diabetics. In addition, sucralose cannot be utilized by dental caries bacteria and will not cause dental caries. It has been approved as a food sweetener by more than 20 countries. ...

Claims

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Application Information

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IPC IPC(8): C07H5/02
Inventor 蔡志刚林道兵刘德铭
Owner DAFENG HEGNO PHARMA
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