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Purification method of D-leucine

A purification method, leucine technology, applied in the field of D-leucine purification, can solve the problems of unqualified extracts, high extraction cost, large organic waste water, etc., achieve good separation and purification effect, accelerate crystallization speed, crystallization fast effect

Active Publication Date: 2019-10-15
JING JING PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] Aiming at the problems of large amount of organic solvent used in the purification of D-leucine in the existing fermentation broth, the extract does not meet the requirements of food grade, the extraction cost is high, the method is complicated, and a large amount of organic waste water and other pollutants are produced, the present invention provides a D-leucine Purification method of leucine

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] Take a volume of 135 L of D-leucine fermentation broth and heat it up to 80°C. Under stirring, keep warm for half an hour for inactivation treatment. Acid 3.05kg, control the material temperature below 40°C, pressure below 0.65MPa, flow rate 200L / h through ceramic filtration, remove bacteria residue and some impurities, collect a total of 117L of ceramic filtrate, take a sample to detect the concentration of D-leucine in the filtrate is 22.97 g / L, total D-leucine 2.69kg.

[0032] Adjust the pH of the obtained Tao filtrate to 5.5, concentrate at 60°C to obtain a concentrated solution, make the concentration of D-leucine in the concentrated solution reach 100g / L, add NaCl to the concentrated solution, and adjust the ionic strength in the concentrated solution After reaching 0.2mol / L, carry out gradient cooling at a cooling rate of 8°C / h until the temperature of the concentrated solution drops below 15°C, and crystallize to obtain 3.48kg of D-leucine wet powder;

[0033] ...

Embodiment 2

[0036] Take a volume of 135L of D-leucine fermentation broth and heat it up to 80°C. Under stirring, keep it warm for half an hour for inactivation treatment. After the treatment, take a sample to detect that the D-leucine content is 41.89g / L. Acid 5.65kg, control material temperature below 40°C, pressure below 0.65MPa, flow rate 220L / h through pottery filter, remove bacteria residue and some impurities, collect a total of 120L pottery filtrate, take samples to detect the concentration of D-leucine in the filtrate is 40.91 g / L, a total of 4.91kg of D-leucine.

[0037] Adjust the pH of the obtained Tao filtrate to 6, concentrate at 70°C to obtain a concentrated solution, make the concentration of D-leucine in the concentrated solution reach 110g / L, add NaCl to the concentrated solution, and adjust the ionic strength in the concentrated solution After reaching 0.25mol / L, carry out gradient cooling at a cooling rate of 9°C / h until the temperature of the concentrated solution drop...

Embodiment 3

[0041] Take a volume of 135 L of D-leucine fermentation broth and heat it up to 80°C. Under stirring, keep warm for half an hour for inactivation treatment. After the treatment, take a sample to detect that the D-leucine content is 43.1g / L. Acid 5.81kg, control material temperature below 40°C, pressure below 0.65MPa, flow rate 250L / h through pottery filter, remove bacteria residue and some impurities, collect a total of 121L pottery filtrate, take samples to detect the concentration of D-leucine in the filtrate is 43.26 g / L, a total of 5.23kg of D-leucine.

[0042] Adjust the pH of the obtained Tao filtrate to 6.5, concentrate at 80°C to obtain a concentrated solution, make the concentration of D-leucine in the concentrated solution reach 120g / L, add NaCl to the concentrated solution, and adjust the ionic strength in the concentrated solution After reaching 0.3mol / L, carry out gradient cooling at a rate of 10°C / h until the temperature of the concentrated solution drops below 1...

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PUM

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Abstract

The invention relates to the technical field of amino acid purification, and particularly discloses a purification method of D-leucine. The purification method comprises the following steps: a, filtering to remove bacteria in D-leucine fermentation liquor to obtain filtrate; b, regulating the pH value of the filtrate to 5.5-6.5, concentrating the filtrate, adding inorganic salt until the ion strength in the concentrated solution reaches 0.2-0.3 mol / L, and cooling the concentrate to obtain D-leucine coarse powder; and c, dissolving the D-leucine crude powder in an aqueous solution with the pH value of 9.5-10.5, adding an acid to adjust the pH value to 5.5-6.5, adding an inorganic salt until the ion strength in the mixed solution reaches 0.05-0.1 mol / L, carrying out cooling crystallization,and filtering and drying the mixture to obtain the D-leucine crystal. The purification method of the D-leucine is simple, high in speed, good in effect, free of organic wastewater discharge, low in cost and simple in equipment requirement, and the obtained D-leucine crystal satisfies the food-grade requirement.

Description

technical field [0001] The invention relates to the technical field of amino acid purification, in particular to a method for purifying D-leucine. Background technique [0002] Amino acids are the basic units of biologically functional macromolecular proteins, which can be synthesized in plant or animal tissues, and can also be obtained by protein hydrolysis. They play an important role in the metabolism, growth, maintenance and repair of tissues. As an important nutrient, amino acids can be obtained from food without supplementing by other supplementary means. However, in special cases, in order to restore the metabolic balance in the body and enhance immunity, it is necessary to supplement various amino acids. [0003] Leucine, isoleucine, and valine are branched-chain amino acids that aid in post-workout muscle recovery, control blood sugar, and provide energy to body tissues. Among them, D-leucine is the most effective branched-chain amino acid, but the human body canno...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C227/40C07C229/08
CPCC07C227/40C07B2200/07C07C229/08
Inventor 闫孟姣何连顺李斌水
Owner JING JING PHARMA