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Method for purifying lactulose by supersaturation deep-induced crystallization

A technology for inducing crystallization and lactulose, applied in chemical instruments and methods, disaccharides, sugar derivatives, etc., can solve the problems of high pressure in large-scale production, difficult removal of monosaccharides, excessive monosaccharides, etc., and achieve efficient crystallization and separation , Scientific and reasonable design, effective purification effect

Inactive Publication Date: 2020-05-08
JIANGSU HI STONE PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Among them, the conventionally converted lactulose mixture cannot meet the standards of pharmaceuticals; although the conversion of chemical methods is relatively high, complex processes such as column chromatography to remove boron have greatly increased the pressure on environmental protection, and the cost is high, and the pressure on large-scale production is great; Biological conversion is relatively mild, environmental protection pressure and post-processing are relatively simple, and it is the most promising solution in the future
However, due to its relatively low conversion rate, the conversion rate of most conversion reactions is 60-80%, and the lactose content is about 20%, which cannot meet the requirements of drug quality standards.
[0006] Lactose is the most difficult miscellaneous sugar in the conversion. Once the conversion rate of lactose is increased, it will inevitably cause the chain-breaking hydrolysis of lactose and the already formed lactulose, thereby forming small molecules of galactose and fructose, resulting in excessive monosaccharides, and These small molecule monosaccharides are more difficult to remove
Due to the above reasons, the most promising bio-enzyme conversion method cannot be effectively applied to the production of lactulose drugs on a large scale
[0007] At present, there are very few methods for reducing lactose in lactulose reported in the literature. Generally, they are separated by columns, which is inefficient and expensive, and cannot be applied industrially.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] Take 200g of a lactulose solution to be separated with a mass percentage of lactose of 20%, a water mass percentage of 23%, and a solution density of 1.30g / ml, at a temperature below 20-30°C, at a speed of 15-30r / min Stir at high speed, add 138g of ethanol with a volume concentration of 95%, stir for 5 minutes until uniform, add 20g of lactose as an induced crystal nucleus, stir for 15 minutes, slow down the stirring speed to 5~10r / min, continue stirring and crystallizing for 72 hours , and then cooled to below 20°C, settled by a sedimentation centrifuge, filtered to remove the precipitated lactose, and the filtrate was evaporated to remove ethanol under reduced pressure to obtain concentrated and distilled lactulose concentrated solution, which was analyzed by differential detection by HPLC. The mass percentage content of lactulose is 8.5%, and the mass percentage content of lactulose is ≥75%. The finished product yield is 85%, which meets the requirements of drug qual...

Embodiment 2

[0031] Take 200g of a lactulose solution to be separated with a mass percentage of lactose of 20%, a water mass percentage of 23%, and a solution density of 1.30g / ml, at a temperature of 45~60°C and a pressure of 3~8MPa. Concentrate under reduced pressure to remove 20-25g of water, cool the concentrated solution to 20-30°C, add 30g of lactose crystals under continuous stirring at a speed of 5-10r / min, keep stirring and crystallizing below 30°C for 48 hours, then Sediment through a sedimentation centrifuge, filter out the precipitated lactose, and the filtrate is a concentrated lactulose solution. After differential detection and analysis by HPLC, the mass percentage of lactose in the lactulose concentrated solution is 6.5-8.0%, and the mass percentage of lactulose ≥75%. The yield of lactulose finished product is 80%, meeting the requirements of pharmaceutical quality standards.

Embodiment 3

[0033] Take 272g of a lactulose solution to be separated with a mass percentage of lactose of 20%, a water mass percentage of 23%, and a solution density of 1.30g / ml. Stir, add 54.5g of lactose crystals, keep stirring and crystallizing below 30°C for 48 hours, then settle through a sedimentation centrifuge, filter and remove the precipitated lactose crystals, and the obtained filtrate is a lactulose concentrated solution, which is analyzed by HPLC differential detection. Lactulose The mass percent content of lactose in the concentrated solution is 8.5-10.0%, and the yield of lactulose finished product is 83-85%, meeting the requirements of pharmaceutical quality standards.

[0034] The principle of a method of supersaturation depth induced crystallization and purification of lactulose in the present invention is to use the solubility difference between lactulose and lactose in the same solvent system to artificially create a supersaturated solution system and create an excessiv...

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Abstract

The invention discloses a method for purifying lactulose by supersaturation deep-induced crystallization. The method comprises the following steps: firstly, converting lactose in a lactulose solutioninto a supersaturation state, then adding lactose crystals to induce crystallization, and finally, performing sedimentation by a sedimentation centrifuge to crystallize and remove all lactose by filtering to obtain a purified lactulose solution. The method for purifying the lactulose by supersaturation deep-induced crystallization is scientific and reasonable in design. The lactose in the lactulose solution is in a supersaturation state, then the lactose is used as a crystal nucleus to induce crystallization, so that efficient crystallization separation of the lactose is achieved, the lactoseis effectively separated from the lactulose, and the lactulose is effectively purified.

Description

technical field [0001] The invention relates to the technical field of lactulose purification, in particular to a method for crystallization and purification of lactulose induced by supersaturation depth. Background technique [0002] The chemical name of lactulose is 4-O-β-D-galactopyranosyl-D-fructose, which is a disaccharide composed of galactose and fructose that does not exist in nature. It is produced artificially by chemical or biological methods A lactulose sugar formed by isomerizing lactose. [0003] Due to the many side reactions in the process of isomerization of lactose, the selectivity of the conversion reaction is not strong, and five possible isomer disaccharides and more than two kinds of monosaccharides are formed during the entire conversion process. In order to better control the formation ratio of various miscellaneous sugars and better obtain lactulose, it is necessary to control the corresponding conversion conditions and time and other factors. In a...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07H3/04C07H1/06
CPCC07H1/06C07H3/04
Inventor 杨宇卫耿虎陈星夏晓霞孙征宇
Owner JIANGSU HI STONE PHARMA