A kind of organically synthesized carboxymethyllysine separation and purification method

A carboxymethyl lysine, separation and purification technology, which is applied in the field of silica gel column chromatography separation and purification for synthesizing carboxymethyl lysine, can solve the problems of low efficiency and cumbersome ion exchange chromatography separation and purification methods, and achieves improved purification. Efficiency, the effect of reducing the experimental cost

Active Publication Date: 2016-08-24
WUHAN POLYTECHNIC UNIVERSITY
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Problems solved by technology

At present, the separation and purification methods of preparative liquid chromatography and ion exchange chromatography reported in the literature are cumbersome and inefficient. Exploring fast, efficient and low-cost separation and purification methods has become the key to obtaining a large amount of low-cost and high-purity carboxymethyllysine monomers.

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  • A kind of organically synthesized carboxymethyllysine separation and purification method
  • A kind of organically synthesized carboxymethyllysine separation and purification method
  • A kind of organically synthesized carboxymethyllysine separation and purification method

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Embodiment

[0060] Reductive amination reaction: Weigh 1.88g (10mmol) of N-acetyl-L-lysine and 1.47g (20mmol) of glyoxylic acid monohydrate into a 250mL round bottom flask and add 80mL of 0.1mol / L Na 2 CO 3 Solution dissolved, continue to add 6.5g reducing agent NaBH 3 CN was placed in the reaction system, after the air in the reaction device was evacuated, nitrogen protection was introduced, and the reaction was carried out at 37°C for 20h. .

[0061] Esterification reaction: After the reaction is over, slowly add enough 37% concentrated hydrochloric acid to the reaction solution to remove excess unreacted NaBH 3CN, concentrated under reduced pressure in vacuo, and recovered the solvent to dryness. Add 40 mL of 3 mol / L hydrochloric acid n-butanol solution to dissolve the dried residue, mix well, and vacuum filter through a 0.45 μm organic filter to remove undissolved salt. The obtained clear solution was reacted at 65°C for 2h under constant stirring. After the reaction was complete...

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Abstract

The invention provides a separating purification method of organically synthesized carboxy methyl lysine. Separating purification is a key step for finally obtaining high-purity carboxy methyl lysine; preparative liquid chromatography and ion exchange chromatography separating purification methods are used at present in the prior art and these methods are relatively cumbersome, low in efficiency and not suitable for mass preparation. To explore quick, efficient and low-price separating purification method becomes very important for obtaining a large quantity of low-cost high-purity carboxy methyl lysine monomers. The separating purification method of carboxy methyl lysine is innovated boldly in the invention, the synthesis amount of carboxy methyl lysine is improved to the gram grade, the purification efficiency of carboxy methyl lysine is increased greatly, the experiment cost is lowered, and a foundation is further laid for carrying out various toxicological evaluations on carboxy methyl lysine.

Description

technical field [0001] The invention belongs to the field of chemical synthesis and its separation and purification, and in particular relates to a silica gel column chromatography separation and purification method for synthesizing carboxymethyllysine. Background technique [0002] In recent years, carboxymethyllysine has become a hot research topic in food processing safety. Due to the difficulty in accurately detecting the content of carboxymethyllysine in different kinds of foods, most studies focus on the establishment and verification of carboxymethyllysine detection methods and the formation reasons of carboxymethyllysine in food , inhibition method, content detection and analysis, etc. As a compound widely present in food, the toxicological evaluation of carboxymethyllysine has not been carried out, and the toxicological data is relatively lacking. At present, the research on the harm of carboxymethyllysine is mainly concentrated in the field of physiology and medi...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C227/40C07C229/26
Inventor 宫智勇柳鑫吴永宁张荣刘亮
Owner WUHAN POLYTECHNIC UNIVERSITY
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