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Clean method for producing high-purity laminine

A technology of laminin and its production method, which is applied in the field of clean production of high-purity laminin, and can solve problems such as affecting product purity, increasing by-products, and overloading of single-stage ion exchange columns.

Inactive Publication Date: 2007-04-25
QINGDAO UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the method still has the defects that the purity of lamininine is not high and it is difficult to control
The main reason is that a strong base such as sodium hydroxide is used as a pH regulator in the complex reaction of L-lysine and heavy metal ions to form a complex. On the one hand, it is difficult to control the pH value within a suitable range during the reaction. On the other hand, sodium hydroxide easily forms insoluble salts with heavy metal ions
Insoluble salts are not only mixed in the reaction system, it is difficult to remove and affect the purity of the product, but also the α-amino masking reaction of L-lysine is not complete, so that the increase of by-products also affects the purity of the product
[0005] Furthermore, the Chinese invention patent CN200410024504.3 uses a single-stage ion exchange column to separate and purify the mixed system of lamininic acid products, because the mixed system contains insoluble metal hydroxides, unreacted lysine raw materials, and metal ammonia carboxyl complexes , monomethylated lysine, dimethylated lysine, esterified lysine, soluble inorganic salts and other impurities make the single-stage ion exchange column multifunctional and overloaded, so the purification effect is poor , the product purity cannot reach more than 98%

Method used

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  • Clean method for producing high-purity laminine
  • Clean method for producing high-purity laminine
  • Clean method for producing high-purity laminine

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] In a 100L reaction kettle, first add 70 kg of distilled water, add 18 kg of L-lysine hydrochloride into the reaction kettle under stirring and dissolve completely, then add ammonia water to adjust the pH value to 7, then slowly add 25 kg of zinc sulfate , React at a constant temperature of 60°C for 1, 1.5 or 2 hours to allow lysine to react completely with zinc ions; then react with 28 kg of dimethyl carbonate to obtain a mixed solution of laminin.

[0027] Pass the laminin complex mixed solution through a strongly acidic cation resin exchange column to adsorb the laminin complex, and wash to remove impurities such as lysine, monomethylated lysine, and dimethylated lysine.

[0028] Add 14 kg of ethylenediaminetetraacetic acid disodium salt to the laminamic acid complex solution obtained by desorption to produce a metal ion demasking reaction to obtain a laminamic acid mixed solution, and pass the mixed solution through the second strongly acidic cation resin exchange col...

Embodiment 2

[0030] In a 500L reactor, first add 360 kg of distilled water, add ammonia water to adjust the pH value to 9, add 95 kg of L-lysine hydrochloride to the reactor to dissolve under stirring, add ammonia water to adjust the pH value to 9, 10 or 11. Add 105 kg of zinc sulfate and react at a constant temperature of 60°C for 1, 1.5 or 2 hours to allow lysine to react completely with zinc ions; then react with 121 kg of dimethyl carbonate to obtain a mixed solution of laminin.

[0031] Pass the laminin complex mixed solution through a strongly acidic cation resin exchange column to adsorb the laminin complex, and wash to remove impurities such as lysine, monomethylated lysine, and dimethylated lysine.

[0032] Add 72 kg of ethylenediaminetetraacetic acid disodium salt to the laminamic acid complex solution obtained by desorption to produce a metal ion demasking reaction to obtain a laminamic mixed solution, and pass the mixed solution through the second strongly acidic cation resin ex...

Embodiment 3

[0034] In a 500L reactor, first add 360 kg of distilled water, add ammonia water to adjust the pH value to 11, add 95 kg of L-lysine hydrochloride into the reactor to dissolve under stirring, add ammonia water to adjust the pH value to 9, 10 or 11. Add 105 kg of zinc sulfate and react at a constant temperature of 60°C for 1, 1.5 or 2 hours to allow lysine to react completely with zinc ions; then react with 121 kg of dimethyl carbonate to obtain a mixed solution of laminin.

[0035] Pass the laminin complex mixed solution through a strongly acidic cation resin exchange column to adsorb the laminin complex, and wash to remove impurities such as lysine, monomethylated lysine, and dimethylated lysine.

[0036] Add 72 kg of ethylenediaminetetraacetic acid disodium salt to the laminamic acid complex solution obtained by desorption to produce a metal ion demasking reaction to obtain a laminamic mixed solution, and pass the mixed solution through the second strongly acidic cation resin...

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Abstract

The invention discloses a cleaning manufacturing method of high-purity laminine, which is characterized by the following: adopting lysine as raw material; reacting lysine with metal salt under alkaline condition (pH =7-11) to do alpha-amino shelter reaction to generate intermediate product; reacting with methylating agent to produce quaternised lysine derivant on the yimxilong-amino; generating metal ionic demasking reaction with complexing agent to obtain rough product of N-trimethyl lysine; adsorbing through cationic resin exchange column; washing; purifying to obtain the product; making ammonia as adjuster of pH value.

Description

technical field [0001] The present invention relates to a clean production method of high-purity laminin. Specifically, non-toxic, environment-friendly chemical raw materials and special process conditions are used in the whole preparation process of laminin, which not only ensures that laminin can be used as medicine or Quality requirements for food additives, and at the same time truly ensure that laminin is a green product. Background technique [0002] Kelp contains a non-protein amino acid with special physiological effects, that is, N-trimethyllysine. Because kelp is another name for kelp, N-trimethyllysine is also called laminin. Laminin has a special effect of lowering blood pressure. It can prevent the occurrence of hypertension and cerebral hemorrhage by lowering cholesterol, lowering blood fat, and preventing atherosclerosis. Therefore, laminin is a green cardiovascular and cerebrovascular API that is safe for the human body. [0003] The content of laminin in k...

Claims

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Application Information

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IPC IPC(8): C07C229/26C07C227/16C07C227/40
Inventor 李群彭衍磊
Owner QINGDAO UNIV
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