CN112624933A - Preparation method of branched chain amino acid chelated copper - Google Patents
Preparation method of branched chain amino acid chelated copper Download PDFInfo
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- CN112624933A CN112624933A CN202011626141.6A CN202011626141A CN112624933A CN 112624933 A CN112624933 A CN 112624933A CN 202011626141 A CN202011626141 A CN 202011626141A CN 112624933 A CN112624933 A CN 112624933A
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- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C227/00—Preparation of compounds containing amino and carboxyl groups bound to the same carbon skeleton
- C07C227/14—Preparation of compounds containing amino and carboxyl groups bound to the same carbon skeleton from compounds containing already amino and carboxyl groups or derivatives thereof
- C07C227/18—Preparation of compounds containing amino and carboxyl groups bound to the same carbon skeleton from compounds containing already amino and carboxyl groups or derivatives thereof by reactions involving amino or carboxyl groups, e.g. hydrolysis of esters or amides, by formation of halides, salts or esters
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Abstract
The invention discloses a preparation method of branched chain amino acid chelated copper, which comprises the following steps: adding raw materials into a high-pressure reaction kettle; heating the high-pressure reaction kettle to raise the temperature to obtain a reaction solution; putting the reaction liquid into a crystallization kettle for cooling crystallization; centrifuging and drying the crystal liquid; crushing the dried product, and placing the crushed product into a sterilization box for sterilization; packaging to obtain food grade branched chain amino acid copper, wherein the branched chain amino acid is food grade valine, leucine, isoleucine or mixture thereof. The invention has the beneficial effects that: according to the invention, the branched chain amino acid is food grade valine, leucine, isoleucine and a mixture thereof, the copper source is food grade copper hydroxide, copper oxide and a mixture of the food grade copper hydroxide and the copper oxide, the mixture is stirred, mixed and heated at high temperature in a high-pressure reaction kettle, the post-treatment adopts cooling crystallization, centrifugal drying and sterilization operation, the process is fine and complete, and the quality of the obtained branched chain amino acid chelated copper is higher.
Description
Technical Field
The invention relates to branched chain amino acid chelated copper, in particular to a preparation method of branched chain amino acid chelated copper, and belongs to the technical field of copper supplement preparations.
Background
Of the 9 essential amino acids required by the human body, 3 are called Branched Chain Amino Acids (BCAAs): leucine, isoleucine and valine. Leucine is a signal for starting muscle protein synthesis, isoleucine is beneficial to the formation of hemoglobin, and has the effects of stabilizing and regulating blood sugar and heat utilization, and valine prevents muscle loss and provides more extra energy for muscle to generate glucose. Copper is a trace nutrient element necessary for human bodies, although the content of copper in the human bodies is very low, the copper is distributed in tissues and organs of the whole body, the hematopoietic function of the human bodies can be promoted, hair is promoted to be brighter, the development and the function of skin, skeletal tissues, internal organs such as brain, liver, heart and the like are all greatly influenced, for a body builder, the copper is more important than the copper thought by people in the past, the copper not only participates in the transportation and utilization of oxygen, but also participates in the reaction of various enzymes, the most important one is beneficial to the generation of norepinephrine, the copper can also increase the blood volume of muscles when high-strength exercise is carried out, people not only need branched chain amino acid and trace element copper in the process of muscle building, and people need a product which supplements both branched chain amino acid and trace element, but also have the following defects in the existing copper supplement product:
the existing copper supplement product and branched chain amino acid are single products, and are not perfectly combined products, two products need to be supplemented simultaneously in actual life, so that the copper supplement product and the branched chain amino acid are inconvenient, the proportion is complex, the control is difficult, and the absorption effect of a human body is poor.
Disclosure of Invention
The present invention has been made to solve the above problems, and an object of the present invention is to provide a method for producing copper chelated with a branched amino acid.
The invention achieves the aim through the following technical scheme, and provides a preparation method of branched chain amino acid chelated copper, which comprises the following steps:
(1) adding raw materials into a high-pressure reaction kettle;
(2) heating the high-pressure reaction kettle to raise the temperature to obtain a reaction solution;
(3) cooling and crystallizing the reaction liquid in a crystallization kettle;
(4) centrifuging and drying the crystal liquid;
(5) crushing and sieving the dried product, and putting the product into a sterilization box for sterilization;
(6) packaging to obtain the food-grade branched chain amino acid copper.
Preferably, the raw material in the step (1) comprises branched chain amino acid, copper source and water.
Preferably, the branched chain amino acids are food grade valine, leucine, isoleucine and mixtures thereof.
Preferably, the copper source is food grade copper hydroxide and copper oxide and mixtures thereof.
Preferably, the molar ratio of the branched-chain amino acid to the copper source is 2:0.8-2:1.2, and the mass ratio of the branched-chain amino group to the water is 1:4-1: 10.
Preferably, the reaction temperature in the step (2) is 80-220 ℃, and the reaction time is 2-18 hours.
Preferably, the product in step (5) is dried by boiling while drying, and the dried product is crushed and sieved.
Preferably, the sterilization box in the step (5) is sterilized by using an ultraviolet sterilization lamp, and a stirring device is used for stirring during sterilization.
The invention has the beneficial effects that: according to the invention, the branched chain amino acid is food grade valine, leucine, isoleucine and a mixture thereof, the copper source is food grade copper hydroxide, copper oxide and a mixture of the food grade copper hydroxide and the copper oxide, the mixture is stirred, mixed and heated at high temperature in a high-pressure reaction kettle, the post-treatment adopts cooling crystallization, centrifugal drying and sterilization operation, the process is fine and complete, the quality of the obtained branched chain amino acid chelated copper is higher, and the effects of supplementing the branched chain amino acid and trace elements are realized.
Drawings
FIG. 1 is a flow chart of a method of the present invention;
FIG. 2 is an infrared spectrum of copper valine obtained in the first example;
FIG. 3 is an infrared spectrum of copper leucine prepared in example two;
FIG. 4 is an infrared spectrum of isoleucine copper obtained in example III;
FIG. 5 is an infrared spectrum of BCAA (2:1:1) prepared in example three.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The first embodiment is as follows:
referring to fig. 1-2, an embodiment of the present invention is shown: a preparation method of branched chain amino acid chelated copper comprises the following steps:
(1) adding raw materials into a high-pressure reaction kettle;
(2) heating the high-pressure reaction kettle to raise the temperature to obtain a reaction solution;
(3) cooling and crystallizing the reaction liquid in a crystallization kettle;
(4) centrifuging and drying the crystal liquid;
(5) crushing and sieving the dried product, and putting the product into a sterilization box for sterilization;
(6) packaging to obtain the food-grade branched chain amino acid copper.
Specifically, the raw materials in the step (1) comprise branched chain amino acid, a copper source and water.
Specifically, the branched-chain amino acid is food-grade valine.
Specifically, the copper source is food-grade copper hydroxide.
Specifically, the molar ratio of the branched-chain amino acid to the copper source is 2: 1.02, the mass ratio of the branched amino group to the water is 1: 5.
specifically, the reaction temperature in the step (2) is 90 ℃, and the reaction time is 8 hours.
Specifically, the crystals separated in the step (5) are dried by boiling, wherein the yield of copper valine is 88.7%, and the copper content is 21.13%.
Specifically, in the step (5), the sterilization box is sterilized by using an ultraviolet sterilization lamp, and a stirring device is used for stirring during sterilization.
After the infrared spectrum identification, the infrared absorption spectrogram shows that the characteristic absorption peak of N-H in valine undergoes a blue shift, which indicates that the N atom in valine participates in the reaction, and further indicates that the valine and copper undergo a chelation reaction.
Example two:
referring to fig. 1-3, an embodiment of the present invention is shown: a preparation method of branched chain amino acid chelated copper comprises the following steps:
(1) adding raw materials into a high-pressure reaction kettle;
(2) heating the high-pressure reaction kettle to raise the temperature to obtain a reaction solution;
(3) cooling and crystallizing the reaction liquid in a crystallization kettle;
(4) centrifuging and drying the crystal liquid;
(5) crushing and sieving the dried product, and putting the product into a sterilization box for sterilization;
(6) packaging to obtain the food-grade branched chain amino acid copper.
Specifically, the raw materials in the step (1) comprise branched chain amino acid, a copper source and water.
Specifically, the branched chain amino acid is food-grade leucine.
Specifically, the copper source is food grade copper oxide.
Specifically, the molar ratio of the branched-chain amino acid to the copper source is 2: 1.03, the mass ratio of the branched amino group to the water is 1: 8.
specifically, the reaction temperature in the step (2) is 160 ℃, and the reaction time is 4 hours.
Specifically, the crystal separated in the step (5) is dried by boiling, and the dried product is crushed and sieved, wherein the yield of copper leucine is 89.6%, and the copper content is 19.28%.
Specifically, in the step (5), the sterilization box is sterilized by using an ultraviolet sterilization lamp, and a stirring device is used for stirring during sterilization.
After the branched chain amino acid copper leucine prepared in the embodiment is identified by an infrared absorption spectrum, it can be seen from an infrared absorption spectrogram that characteristic absorption peaks of amino groups and carboxyl groups in leucine are shifted, so that the amino groups and the carboxyl groups in the leucine and copper are subjected to a chelation reaction.
Example three:
referring to fig. 1-4, an embodiment of the present invention is shown: a preparation method of branched chain amino acid chelated copper comprises the following steps:
(1) adding raw materials into a high-pressure reaction kettle;
(2) heating the high-pressure reaction kettle to raise the temperature to obtain a reaction solution;
(3) cooling and crystallizing the reaction liquid in a crystallization kettle;
(4) centrifuging and drying the crystal liquid;
(5) and crushing and sieving the dried product, and putting the product into a sterilization box for sterilization.
(6) Packaging to obtain food-grade branched chain copper amino acid;
specifically, the raw materials in the step (1) comprise branched chain amino acid, a copper source and water.
Specifically, the branched chain amino acid is food-grade isoleucine.
Specifically, the copper source is a mixture of food-grade copper hydroxide and copper oxide.
Specifically, the molar ratio of the branched-chain amino acid to the copper source is 2: 0.98, the mass ratio of branched amino groups to water is 1: 6.
specifically, the reaction temperature in the step (2) is 200 ℃, and the reaction time is 4 hours.
Specifically, the crystal separated in the step (5) is dried by boiling, and the dried product is crushed and sieved, wherein the yield of isoleucine copper is 91.5%, and the copper content is 18.96%.
Specifically, in the step (5), the sterilization box is sterilized by using an ultraviolet sterilization lamp, and a stirring device is used for stirring during sterilization.
After the branched chain amino acid copper isoleucine prepared in the embodiment is identified by infrared absorption spectrum, an infrared absorption spectrogram shows that characteristic absorption peaks of amino groups and carboxyl groups of isoleucine are shifted, so that the amino groups and the carboxyl groups in isoleucine are subjected to chelation reaction with copper.
Example four:
referring to fig. 1-5, an embodiment of the present invention is shown: a preparation method of branched chain amino acid chelated copper comprises the following steps:
(1) adding raw materials into a high-pressure reaction kettle;
(2) heating the high-pressure reaction kettle to raise the temperature to obtain a reaction solution;
(3) cooling and crystallizing the reaction liquid in a crystallization kettle;
(4) centrifuging and drying the crystal liquid;
(5) and crushing and sieving the dried product, and putting the product into a sterilization box for sterilization.
(6) Packaging to obtain the food-grade branched chain amino acid copper.
Specifically, the raw materials in the step (1) comprise branched chain amino acid, a copper source and water.
Specifically, the branched chain amino acid is food-grade leucine, valine and isoleucine in a mass ratio of 2:1: 1.
specifically, the copper source is food-grade copper hydroxide.
Specifically, the molar ratio of the branched-chain amino acid to the copper source is 2: 1.05, the mass ratio of the branched amino group to the water is 1: 8.
specifically, the reaction temperature in the step (2) is 220 ℃, and the reaction time is 4 hours.
Specifically, the crystal separated in the step (5) is dried by boiling, and the dried product is crushed and sieved, wherein the yield of the branched chain copper amino acid is 85.4%, and the copper content is 19.92%.
Specifically, in the step (5), the sterilization box is sterilized by using an ultraviolet sterilization lamp, and a stirring device is used for stirring during sterilization.
After the copper branched amino acid prepared in the embodiment is identified by infrared absorption spectrum, the infrared absorption spectrum shows that the copper branched amino acid and the copper have a chelation reaction.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential attributes thereof. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein. Any reference sign in a claim should not be construed as limiting the claim concerned.
Furthermore, it should be understood that although the present description refers to embodiments, not every embodiment may contain only a single embodiment, and such description is for clarity only, and those skilled in the art should integrate the description, and the embodiments may be combined as appropriate to form other embodiments understood by those skilled in the art.
Claims (8)
1. A preparation method of branched chain amino acid chelated copper is characterized by comprising the following steps: the preparation method of the branched chain amino acid chelated copper comprises the following steps:
(1) adding raw materials into a high-pressure reaction kettle;
(2) heating the high-pressure reaction kettle to raise the temperature to obtain a reaction solution;
(3) cooling and crystallizing the reaction liquid in a crystallization kettle;
(4) centrifuging and drying the crystal liquid;
(5) crushing and sieving the dried product, and putting the product into a sterilization box for sterilization;
(6) packaging to obtain the food-grade branched chain amino acid copper.
2. The method for producing branched-chain-amino-acid chelated copper according to claim 1, characterized in that: the raw materials in the step (1) comprise branched chain amino acid, a copper source and water.
3. The method for producing branched-chain-amino-acid chelated copper according to claim 2, characterized in that: the branched chain amino acids are food grade valine, leucine, isoleucine and mixtures thereof.
4. The method for producing branched-chain-amino-acid chelated copper according to claim 2, characterized in that: the copper source is food-grade copper hydroxide and copper oxide and a mixture of the food-grade copper hydroxide and the copper oxide.
5. The method for producing branched-chain-amino-acid chelated copper according to claim 2, characterized in that: the molar ratio of the branched chain amino acid to the copper source is 2:0.8-2:1.2, and the mass ratio of the branched chain amino group to the water is 1:4-1: 10.
6. The method for producing branched-chain-amino-acid chelated copper according to claim 1, characterized in that: the reaction temperature in the step (2) is 80-220 ℃, and the reaction time is 2-18 hours.
7. The method for producing branched-chain-amino-acid chelated copper according to claim 1, characterized in that: and (5) drying the product in the step (5) by boiling, and crushing and sieving the dried product.
8. The method for producing branched-chain-amino-acid chelated copper according to claim 1, characterized in that: and (5) sterilizing the sterilizing box by using an ultraviolet sterilizing lamp, and stirring by using a stirring device during sterilization.
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2020
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