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Method for preparing magnesium L-pyroglutamate

A technology for magnesium pyroglutamate and pyroglutamate, applied in the field of preparing L-magnesium pyroglutamate, which can solve the problems of no process reports, etc., and achieve the effects of simple operation, low cost and proper proportioning

Inactive Publication Date: 2010-10-20
宜兴市前成生物有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] Although magnesium pyroglutamate is widely used, there is no relevant process report at home and abroad

Method used

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  • Method for preparing magnesium L-pyroglutamate
  • Method for preparing magnesium L-pyroglutamate
  • Method for preparing magnesium L-pyroglutamate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Embodiment 1 small test program

[0026] The first step: dehydration to prepare L-pyroglutamic acid

[0027] Feed in a 3L stainless steel reactor: 300g of L-glutamic acid (food grade), 1200ml of deionized water and raise the temperature to 113°C-115°C, maintain it for 9 hours, and the reaction is complete. The coking rate can reach 96%, and the racemization rate can be controlled below 0.5%.

[0028] The second step: separation and extraction of pyroglutamic acid

[0029] After coking, cool the reaction solution to room temperature, add the same volume of deionized water to dilute the original volume twice, and directly put it on the 732 cation exchange resin column prepared in advance to separate L-pyroglutamic acid and uncoked L-glutamic acid .

[0030] The third step: preparation of magnesium L-pyroglutamate

[0031] Add the extracted L-pyroglutamic acid solution in a 5000ml beaker, stir and heat, when the temperature rises to 70°C, add 69g of magnesium carbonate...

Embodiment 2

[0033] Example 2 pilot test program

[0034] The first step: dehydration to prepare L-pyroglutamic acid

[0035] Feed in a 2-ton stainless steel reactor: L-glutamic acid (food grade) 300kg, deionized water 1500L, heat up to 116°C-118°C, maintain for 8 hours, and the reaction is complete. The coking rate can reach 96%, and the racemization rate can be controlled below 0.5%.

[0036] The second step: Separation and extraction of L-pyroglutamic acid

[0037] After coking, cool the reaction solution to room temperature, add deionized water to dilute the original volume by 2.5 times, and directly put it on the 732 cation exchange resin column prepared in advance to separate L-pyroglutamic acid and uncoked L-glutamic acid. The isolated L-pyroglutamic acid NMR spectrum is shown in figure 1 .

[0038] The third step: preparation of magnesium L-pyroglutamate

[0039] Add the extracted L-pyroglutamic acid solution in a 5-ton enamel batching tank, stir and heat, and when the tempera...

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Abstract

The invention discloses a method for preparing magnesium L-pyroglutamate. The preparation process is as follows: a, preparing L-pyroglutamic acid by dehydration, wherein L-glutamic acid and deionized water are put into a reaction kettle, stirred, heated to 100 to 128 DEG C and kept at the temperature for 6 to 12 hours; b, separating and extracting the L-pyroglutamic acid, wherein after pyrogenation is finished, the reaction solution is cooled to room temperature, deionized water is added to dilute the reaction solution, and the L-pyroglutamic acid and the non-pyrolyzed L-glutamic acid are separated by a cation exchange resin column; c, preparing the magnesium L-pyroglutamate, wherein the solution of the L-pyroglutamic acid obtained by the step b is stirred and heated and added with magnesium carbonate or magnesium oxide; and d, separating and extracting the magnesium L-pyroglutamate, wherein a sample is made after the reaction solution obtained by the step c is clear to test the pH value of the reaction solution, the pH value of the reaction solution is adjusted to 6.5 to 7.5, the reaction solution is concentrated till supersaturated solution is obtained, the supersaturated solution is stirred and cooled for crystallization, the solution is subjected to vacuum filtration and the crystals are subjected to vacuum drying to obtain the magnesium L-pyroglutamate. The method is simple in operation, high production efficiency and low in cost and is suitable for industrial production.

Description

technical field [0001] The invention relates to a method for preparing magnesium L-pyroglutamate. Background technique [0002] Magnesium L-pyroglutamate is white odorless crystal or powder. Soluble in water, slightly soluble in methanol and ethanol, insoluble in ether. Molecular formula: C 10 h 12 N 2 o 6 Mg, molecular weight: 280.5, structural formula: [0003] [0004] The European Union listed magnesium pyroglutamate and calcium pyroglutamate in 2009: Substances that can be added to foods for special nutritional purposes for specific nutritional purposes. Studies have proved that magnesium pyroglutamate is widely used in food, medicine, beauty and other fields. U.S. Patent (US7001612) discloses a method for alleviating the reduction of electrolyte levels in the human body caused by excessive sweating due to heat stress, that is, combining magnesium pyroglutamate with sodium compounds, potassium compounds, phosphate and zinc glutamate, etc. The substance is pre...

Claims

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Application Information

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IPC IPC(8): C07D207/28
Inventor 席日新李海涛王瑛华
Owner 宜兴市前成生物有限公司
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