阅读说明：本技术 一种饲料添加剂用自主组装小肽螯合铁的制备方法 (Preparation method of self-assembled small peptide chelated iron for feed additive ) 是由 山成明 邓国为 苏义雄 于 2021-08-31 设计创作，主要内容包括：本发明涉及化学合成技术领域,具体为一种饲料添加剂用自主组装小肽螯合铁的制备方法,所述饲料添加剂用自主组装小肽螯合铁的制备方法是首先制备小肽粉,然后通小肽粉与无机碱反应后得到小肽螯合铁,具体包含以下步骤：步骤一,准备制备原材料；步骤二,原材料的添加：将氨基酸放入容器内部,随后加入水源,将氨基酸与水进行充分融合；步骤八,将得到的溶液内部加入甲醇,使其析出小肽螯合铁；步骤九,进行过滤,随后进行借助器械进行干燥,即可得到小肽螯合铁。本发明带来了小肽鳌合铁与可以显著提高仔猪红细胞浓度,从而使得仔猪对铁元素的吸收利用率更高,有效的减少粪便中微量元素的含量,避免对环境造成较大的污染,并且制作过程中操作简单。(The invention relates to the technical field of chemical synthesis, in particular to a preparation method of self-assembled small peptide chelated iron for a feed additive, which comprises the following steps of firstly preparing small peptide powder, and then reacting the small peptide powder with an inorganic base to obtain the small peptide chelated iron: step one, preparing a raw material; step two, adding raw materials: putting amino acid into a container, then adding a water source, and fully fusing the amino acid and the water; step eight, adding methanol into the obtained solution to separate out small peptide chelated iron; and step nine, filtering, and then drying by means of an instrument to obtain the small peptide chelated iron. The invention brings small peptide chelated iron and can obviously improve the concentration of piglet red blood cells, thereby leading the piglet to have higher absorption and utilization rate of iron elements, effectively reducing the content of trace elements in excrement, avoiding larger pollution to the environment and having simple operation in the manufacturing process.)

1. A preparation method of self-assembled small peptide chelated iron for feed additives is characterized by comprising the following steps: the preparation method of the self-assembled small peptide chelated iron for the feed additive comprises the steps of firstly preparing small peptide powder, and then reacting the small peptide powder with inorganic base to obtain the small peptide chelated iron;

the method specifically comprises the following steps:

step one, preparing raw materials: preparing amino acid, strong acid resin and inorganic ferrous solution inorganic base;

step two, adding raw materials: putting amino acid into a container, then adding a water source, and fully fusing the amino acid and the water;

step three, reaction of raw materials: then adding strong acid resin, and stirring under a heating condition to react;

step four, forming material preparation: after the reaction is finished, filtering the raw materials by means of an instrument, filtering strong acid resin by a filtering mode, and drying the raw materials to form small peptide powder;

step five, further preparing the raw materials: dissolving the prepared small peptide powder to obtain a small peptide solution;

step six, reaction of raw materials: adding an inorganic ferrous solution under the condition of heating to fully dissolve the inorganic ferrous solution;

step seven, adding inorganic base into the raw materials after full dissolution to enable the small peptide to react with iron to form a chelate;

step eight, adding methanol into the obtained solution to separate out small peptide chelated iron;

and step nine, filtering, and then drying by means of an instrument to obtain the small peptide chelated iron.

2. The method for preparing self-assembled small peptide chelated iron as feed additive according to claim 1, wherein the method comprises the following steps: the amino acid can be glycine, alanine, valine, leucine, isoleucine, methionine (methionine), proline, tryptophan, serine, tyrosine, cysteine, phenylalanine, asparagine, glutamine, threonine, aspartic acid, glutamic acid, lysine, arginine, histidine and selenocysteine.

3. The method for preparing self-assembled small peptide chelated iron as feed additive according to claim 1, wherein the method comprises the following steps: the amino acid proportion is evenly distributed according to the required components, so that the total concentration of the amino acid is 200 g/L.

4. The method for preparing self-assembled small peptide chelated iron as feed additive according to claim 1, wherein the method comprises the following steps: the mass of the strong acid resin is 5 percent of the weight of the amino acid.

5. The method for preparing self-assembled small peptide chelated iron as feed additive according to claim 1, wherein the method comprises the following steps: the heating condition in the preparation of the small peptide powder was 80 ℃, and it was reacted for 3 hours.

6. The method for preparing self-assembled small peptide chelated iron as feed additive according to claim 1, wherein the method comprises the following steps: the inorganic ferrous solution is 20-25% ferrous sulfate solution.

7. The method for preparing self-assembled small peptide chelated iron as feed additive according to claim 1, wherein the method comprises the following steps: the inorganic alkali is sodium carbonate, and the mass of the inorganic alkali is 3-5% of the sum of the mass of the dry peptide powder and the mass of the ferrous sulfate.

8. The method for preparing self-assembled small peptide chelated iron as feed additive according to claim 1, wherein the method comprises the following steps: the mass ratio of the small peptide to the ferrous sulfate is 3-5:1, the heating condition in the reaction process is 70 ℃, and the reaction time is 1 hour.

Technical Field

The invention relates to the technical field of chemical synthesis, in particular to a preparation method of self-assembled small peptide chelated iron for a feed additive.

Background

Iron is an essential component of human cells, has hematopoietic function, participates in the production of hemoglobin and the synthesis of cytochrome and various enzymes, and promotes growth. Iron also functions to transport and carry nutrients in the blood, and if iron is deficient, people suffer from iron deficiency anemia, and also cause a decrease in immune function and a disturbance in metabolism, as do animals, which contain iron in many tissues.

Iron in animals exists mostly in the form of protein complexes, and participates in substance metabolism and energy metabolism in life activities in various forms. Iron is present in erythrocytes as hemoglobin, in muscles as myoglobin, in serum as transferrin and ferritin, in placenta as uteroferritin, in milk as lactoferrin, and in the liver and spleen as ferritin with a very small proportion being present as divalent or trivalent iron. Iron exists in different forms, and its characteristics and effects are also different. However, iron in any form is necessary for animals, so the iron needs to be supplemented to the animals in the growth process of the animals, and the main method is to add inorganic salt to daily feed for supplementing the animals.

However, such a method is not beneficial for the animal to absorb, so that the animal excrement is discharged together with the animal excrement, and the inorganic salts are not generally treated, so that the environment can be polluted to a certain extent, and certain manpower and material resources are wasted in the subsequent treatment, so that a preparation method of the self-assembled small peptide chelated iron for the feed additive is needed to solve the problems.

Disclosure of Invention

The invention aims to provide a preparation method of self-assembled small peptide chelated iron for a feed additive, which aims to solve the problem that the traditional inorganic salt proposed in the background technology is not beneficial to animal absorption and is discharged along with animal excrement, thereby possibly causing certain pollution to the environment.

In order to achieve the purpose, the invention provides the following technical scheme: a preparation method of self-assembled small peptide chelated iron for feed additives comprises the steps of firstly preparing small peptide powder, and then reacting the small peptide powder with inorganic base to obtain small peptide chelated iron;

the method specifically comprises the following steps:

step one, preparing raw materials: preparing amino acid, strong acid resin and inorganic ferrous solution inorganic base;

step two, adding raw materials: putting amino acid into a container, then adding a water source, and fully fusing the amino acid and the water;

step three, reaction of raw materials: then adding strong acid resin, and stirring under a heating condition to react;

step four, forming material preparation: after the reaction is finished, filtering the raw materials by means of an instrument, filtering strong acid resin by a filtering mode, and drying the raw materials to form small peptide powder;

step five, further preparing the raw materials: dissolving the prepared small peptide powder to obtain a small peptide solution;

step six, reaction of raw materials: adding an inorganic ferrous solution under the condition of heating to fully dissolve the inorganic ferrous solution;

step seven, adding inorganic base into the raw materials after full dissolution to enable the small peptide to react with iron to form a chelate;

step eight, adding methanol into the obtained solution to separate out small peptide chelated iron;

and step nine, filtering, and then drying by means of an instrument to obtain the small peptide chelated iron.

Further, the amino acid may be glycine, alanine, valine, leucine, isoleucine, methionine (methionine), proline, tryptophan, serine, tyrosine, cysteine, phenylalanine, asparagine, glutamine, threonine, aspartic acid, glutamic acid, lysine, arginine, histidine and selenocysteine.

Furthermore, the amino acid proportion is evenly distributed according to the required components, so that the total concentration of the amino acid is 200 g/L.

Further, the mass of the strong acid resin is 5% of the weight of the amino acid.

Further, the heating condition in the preparation of the small peptide powder was 80 ℃, and it was reacted for 3 hours.

Further, the inorganic ferrous solution is 20-25% ferrous sulfate solution.

Further, the inorganic alkali is sodium carbonate, and the mass of the inorganic alkali is 3% -5% of the mass sum of the dry peptide powder and the ferrous sulfate.

Further, the mass ratio of the small peptide to the ferrous sulfate is 3-5:1, the heating condition in the reaction process is 70 ℃, and the reaction time is 1 hour.

Compared with the prior art, the invention has the beneficial effects that:

1. the small peptide chelated iron peptide iron avoids the problem that the traditional inorganic salt is not beneficial to animal absorption and is discharged together with animal excrement, the inorganic salt is not treated generally, so that the environment can be polluted to a certain extent, certain manpower and material resources are wasted during subsequent treatment, the small peptide chelated iron is brought, the red blood cell concentration of piglets can be obviously improved, the absorption and utilization rate of the iron element by the piglets is higher, the small peptide chelated iron and the feed are mixed to be more beneficial to animals to eat, the content of trace elements in the excrement is effectively reduced, the subsequent environment is prevented from being polluted greatly, the operation is simple in the manufacturing process, the requirement on the condition in the reaction process is lower, the overall reaction condition is milder, the preparation is facilitated, the subsequent production and use cost is lower, and the manufacturing is easy.

2. Compared with the existing small peptide preparation technology such as fermentation and condensing agent, the method adopts strong acid resin, and can achieve the advantages of easy separation and purification, easy regeneration and utilization and less three wastes.

3. The small peptide chelate salt has better absorption effect on the traditional inorganic salt and amino acid salt, is not easy to cause the saturation of an absorption channel, can not compete in the absorption between the small peptide chelate salt, is suitable for being mixed with the amino acid chelate salt for use, achieves the secondary supplement effect, and is beneficial to improving the feed utilization rate.

Detailed Description

The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to 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 embodiment provided by the invention comprises the following steps: a preparation method of self-assembled small peptide chelated iron for feed additives comprises the steps of firstly preparing small peptide powder, and then reacting the small peptide powder with inorganic base to obtain small peptide chelated iron;

the method specifically comprises the following steps:

step one, preparing raw materials: preparing amino acid, strong acid resin and inorganic ferrous solution inorganic base;

step two, adding raw materials: putting amino acid into a container, then adding a water source, and fully fusing the amino acid and the water;

step three, reaction of raw materials: then adding strong acid resin, and stirring under a heating condition to react;

step four, forming material preparation: after the reaction is finished, filtering the raw materials by means of an instrument, filtering strong acid resin by a filtering mode, and drying the raw materials to form small peptide powder;

step five, further preparing the raw materials: dissolving the prepared small peptide powder to obtain a small peptide solution;

step six, reaction of raw materials: adding an inorganic ferrous solution under the condition of heating to fully dissolve the inorganic ferrous solution;

step seven, adding inorganic base into the raw materials after full dissolution to enable the small peptide to react with iron to form a chelate;

step eight, adding methanol into the obtained solution to separate out small peptide chelated iron;

and step nine, filtering, and then drying by means of an instrument to obtain the small peptide chelated iron.

The amino acid can be glycine, alanine, valine, leucine, isoleucine, methionine (methionine), proline, tryptophan, serine, tyrosine, cysteine, phenylalanine, asparagine, glutamine, threonine, aspartic acid, glutamic acid, lysine, arginine, histidine and selenium cysteine, adopt this kind of design to be convenient for make the selectivity of material more nimble, make multiple material all can satisfy the demand, do benefit to and select according to the actual demand, make raw and other materials more easily acquire and select, do benefit to follow-up production, make the kind of raw and other materials diversified.

The amino acid proportion is evenly distributed according to the required components, the amino acid is colorless crystal, the melting point is over 200 ℃, and the melting point is much higher than that of common organic compounds. The alpha-amino acid has 4 kinds of tastes of sour, sweet, bitter and fresh. Monosodium glutamate and glycine are the most used umami flavours. Amino acids are generally readily soluble in water, acid solutions and aqueous alkali, and insoluble or slightly soluble in organic solvents such as ethanol or diethyl ether. The amino acids have very different solubilities in water, e.g. tyrosine solubility is minimal, with 100g of tyrosine dissolving only 0.045g in water at 25 ℃, but tyrosine solubility is greater in hot water. Lysine and arginine are often in the form of hydrochloride, because the lysine and the arginine are very soluble in water and difficult to prepare crystals due to deliquescence, so that the total concentration of the lysine and the arginine is 200g/L, and the design is convenient for ensuring that the material proportion is more reasonable and each group of components are the same.

The mass of the strong acid resin is 5% of the weight of the amino acid, the proportion of the amino acid in the reaction process is determined by adopting the design, the problems that the raw material error is large and the production is not facilitated are avoided, and the strong acid resin is a uniform particle resin designed for desalting. Small particle size, homogeneous resins exhibit faster kinetics than conventional particle size resins. Improved kinetics lead to better regeneration efficiency, higher operating exchange capacity, reduced regenerant use, and less wastewater.

The heating condition in the preparation of small peptide powder is 80 deg.C, and the reaction time is 3 hr, the small peptide is generally below 1000 Dalton molecular weight, and is called small peptide, oligopeptide is also called small molecule active peptide. The small peptide is generally an oligopeptide consisting of 2-3 amino acids, the average molecular weight is about 300 daltons, the reaction condition is more suitable by adopting the design, meanwhile, the reaction can be promoted by heating, the time required by the reaction is reduced, the reaction is more sufficient by adopting the reaction time of three hours, and the reaction is avoided being insufficient.

The inorganic ferrous solution is a 20-25% ferrous sulfate solution, and the adoption of the design facilitates the selection of a solution with a proper concentration for reaction, so that the subsequent reaction effect is better, the ferrous sulfate is an inorganic substance and has a chemical formula of FeSO₄The appearance is white powder without smell. The crystalline hydrate is heptahydrate at normal temperature, commonly called as "copperas", light green crystal, weathers in dry air, is oxidized into brown basic ferric sulfate on the surface in humid air, becomes tetrahydrate at 56.6 ℃, and becomes monohydrate at 65 ℃. Ferrous sulfate is soluble in water and almost insoluble in ethanol. The aqueous solution is slowly oxidized in the air when being cooled and is quickly oxidized when being heated. The oxidation can be accelerated by adding alkali or dew. Relative density (d15) 1.897. Has irritation. The ferrous sulfate can be used for chromatographic analysis reagents and drop analysis for measuring platinum, selenium, nitrite and nitrate. Ferrous sulfate can also be used as a reducing agent, for producing ferrites, for purifying water, for polymerizing catalysts, for photomechanical production, etc.

The inorganic alkali is sodium carbonate, the mass of the inorganic alkali is 3% -5% of the mass sum of the dry peptide powder and the ferrous sulfate, the amount of the inorganic alkali can be conveniently determined by adopting the design, the reaction can be carried out according to the appropriate amount determined by actual conditions during the reaction, the sodium carbonate is an inorganic compound, the molecular formula is Na₂CO₃Molecular weight 105.99, also called soda ash, but falls into the category of salts and not bases. Also known as soda or soda ash in international trade. It is an important inorganic chemical raw material, mainly used for producing plate glass, glass products and ceramic glaze. The aqueous solution of sodium carbonate is alkaline and has certain corrosivity, and can generate double decomposition reaction with acid and also can generate double decomposition reaction with calcium salt and barium salt. The solution is alkaline, so that phenolphthalein can turn red.

The mass ratio of the small peptide to the ferrous sulfate is 3-5:1, the heating condition in the reaction process is 70 ℃, the design is adopted to facilitate the determination of the amount of the small peptide and the ferrous sulfate, the selection of a proper ratio for reaction is facilitated, the reaction time is 1 hour, the design is adopted to facilitate the reaction condition to be more proper, and the reaction is more sufficient.

Test examples

The basic diet is prepared according to NRC (2012) pig nutrition requirements in the pig feeding Standard (NY/T65-2004) of China, the basic diet adopts a corn-soybean meal type, and a control group adopts inorganic trace elements (ferrous sulfate heptahydrate) as a nutritional supplement; the experimental group is added with small peptide chelated iron to replace ferrous sulfate heptahydrate with equivalent value, and the composition and various nutritional indexes of the basic feed are shown in the following table

The premix is provided for each kilogram of feed: 100mg of ferrous sulfate heptahydrate/small chelated iron, 60mg of zinc sulfate heptahydrate, 20mg of copper sulfate pentahydrate, 10mg of magnesium sulfate, 0.2mg of potassium iodide, 10mg of manganese sulfate monohydrate, 5400IU of VA, 3110 IU of VD, 15mg of VB, 12mg of citric acid, 7mg of antioxidant, 5mg of chromium picolinate, 280mg of calcium dihydrogen phosphate, 300mg of mountain flour, zeolite powder as a carrier, and ferrous sulfate heptahydrate, commonly called copperas, which is an inorganic compound with a chemical formula of FeSO 4.7H 2O. It is irritant to human respiratory tract, and causes cough and shortness of breath by inhalation. It has irritation to eyes, skin and mucosa. The method is mainly used for manufacturing iron salt, ink, magnetic iron oxide, a water purifying agent, a disinfectant and an iron catalyst; it can be used as coal dyeing agent, tanning agent, bleaching agent, wood preservative, compound fertilizer additive, ferrous sulfate monohydrate, etc.

The nutrient levels are calculated values.

A single-factor test is adopted, wherein 80 healthy piglets with similar weights in 30 +/-1 days are selected and randomly divided into 2 groups, each group is 8 in number of repetitions, each piglet is 10 in number of repetitions, and the 2 kinds of feed are fed respectively, and the test period is 30 days. Grouping of experimental piglets is shown in the following table

Group of	Additive for different iron sources in daily ration
		Control group	Small peptide powder and ferrous sulfate heptahydrate
Test group	Small peptide chelated iron

Measurement indexes are as follows: initial average weight, final average weight, average daily feed intake, average daily gain, and material-to-weight ratio

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.