CN110041213A - A kind of preparation method of glutamate chelate iron - Google Patents
A kind of preparation method of glutamate chelate iron Download PDFInfo
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- CN110041213A CN110041213A CN201910288484.7A CN201910288484A CN110041213A CN 110041213 A CN110041213 A CN 110041213A CN 201910288484 A CN201910288484 A CN 201910288484A CN 110041213 A CN110041213 A CN 110041213A
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- iron
- irradiation
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- glutamate chelate
- chelate iron
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- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23K—FODDER
- A23K20/00—Accessory food factors for animal feeding-stuffs
- A23K20/10—Organic substances
- A23K20/142—Amino acids; Derivatives thereof
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K31/00—Medicinal preparations containing organic active ingredients
- A61K31/185—Acids; Anhydrides, halides or salts thereof, e.g. sulfur acids, imidic, hydrazonic or hydroximic acids
- A61K31/19—Carboxylic acids, e.g. valproic acid
- A61K31/195—Carboxylic acids, e.g. valproic acid having an amino group
- A61K31/197—Carboxylic acids, e.g. valproic acid having an amino group the amino and the carboxyl groups being attached to the same acyclic carbon chain, e.g. gamma-aminobutyric acid [GABA], beta-alanine, epsilon-aminocaproic acid, pantothenic acid
- A61K31/198—Alpha-aminoacids, e.g. alanine, edetic acids [EDTA]
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61P—SPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
- A61P3/00—Drugs for disorders of the metabolism
- A61P3/02—Nutrients, e.g. vitamins, minerals
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- C—CHEMISTRY; METALLURGY
- 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
Abstract
The invention discloses a kind of preparation methods of glutamate chelate iron, and solution is made in glutamic acid and frerrous chloride, carries out electron beam irradiation, separating obtained solid, as glutamate chelate iron.This method has many advantages, such as that easy to operate, the reaction time is short, and the iron in products obtained therefrom is ferrous iron, is not easy to be oxidized ferric iron, can be used as benefit iron new product in livestock and poultry cultivation and plays its effect, ecological environment security is suitable for producing upper large-scale application.
Description
Technical field
The invention belongs to agricultural chemicals technical fields, and in particular to a kind of preparation method of glutamate chelate iron.
Background technique
Iron is one of microelement necessary to organism, plays vital effect.Iron containing in animal body
Amount is generally 30-70mg/kg, average out to 40mg/kg, but with the type of animal, age, gender, health status and nutrition shape
Condition is different and different iron contents is presented.Iron is the important component of hemoglobin in blood rbc, is internal transport oxygen
Main carriers, transferrins is the carrier that oxygen is delivered in body blood circulation, by transferrins with by iron transfer to machine
In each histoorgan of body, to guarantee the normal physiological function of body, iron be the enzymes such as catalase in serum (CAT) composition at
Point, substance in vivo metabolism is participated in, and certain defense reaction is played to body.
The distributional difference of iron is very big in all animal different tissues and organ, and in general, 60%-70% is distributed in blood red
In albumen, 2%-20% is distributed in myoglobins, and 0.1%-0.4% is distributed in cytochromes, and about 1%, which is present in transhipment, carries
In body compound and enzyme system.Piglet, which is born, itself lays in iron 50mg, and daily growth and development needs iron 5-10mg, and sow is daily only
Piglet iron can be supplied less than 5mg, so piglet may generate hypoferric anemia because of the deficiency of iron from 5 ages in days, due to
Sucking pig has the Blank immunization phase in 5-20 age in days or so, so needing to mend iron.Iron in nature is typically all trivalent, and animal is not easy
It is absorbed and utilized.To adding in sow, pig starter feed or though oral ferrous sulfate is ferrous iron, its is oxidizable at ferric iron,
It is absorbable to utilize.At present farm mend iron its be mostly inorganic iron, animal body can only digest and assimilate 10% or so, and ferrous sulfate
It cannot add too much, excessively will affect the digestion of other microelements, absorb.Since over half a century, melt quality additive
It experienced inorganic acid iron, organic acid iron, amino acid chelated iron three phases, with inorganic acid iron, organic acid iron phase ratio, amino acid chela
Closing iron has the advantages that high bioavailability, stability, high-absorbility and safe and non-toxic, therefore amino acid chelated iron is as benefit
Chalybeate has broad application prospects.Amino acid chelated iron is mainly directly synthesized with inorganic divalent iron salt with amino acid at present,
But the ferrous iron exposure of this method preparation is oxidized easily in air, is not easy to prepare stable amino acid in this way
It is chelating ferrous.
Summary of the invention
The purpose of the invention is to overcome drawbacks described above, a kind of preparation method of glutamate chelate iron is provided.
The purpose of the present invention is achieved by the following technical scheme:
A kind of preparation method of glutamate chelate iron, which is characterized in that solution is made in glutamic acid and frerrous chloride, is carried out
Electron beam irradiation, separating obtained solid, as glutamate chelate iron.
Further, the method specifically comprises the following steps:
(1) glutamic acid and frerrous chloride are configured to mixed solution according to molar ratio 1-3:1, adjust pH value to 1.0-6.0
Afterwards, electron beam irradiation 1.0-9.0min is carried out, 20-60 DEG C of irradiation temperature, the dosage of electron beam irradiation is 1.00-3.00kGy；
(2) solution after step (1) irradiation is centrifuged, precipitating is precipitated in mixed solvent, is separated by solid-liquid separation, gained is consolidated
Body be dried to get.
Further, in step (1), the preferred molar ratio of glutamic acid and frerrous chloride is 2:1；
PH value is preferably adjusted to 4, and pH adjusting agent is sodium hydroxide solution；
The electron beam irradiation time is preferably 5min, and irradiation temperature is preferably 40 DEG C, and irradiation dose is preferably 2.50kGy.
Further, in step (2), solvent is 90vt% ethyl alcohol.
The present invention irradiates glutamic acid using the high-energy ray of electron beam, can make to generate in glutamic acid a large amount of free
Base, the free radical in amorphous phase form chelate structure with ferrous ion easily to get glutamate chelate iron is arrived.The chelated iron pair
Piglet has preferable benefit iron effect, can be in piglet cultivates for preventing and curing diseases, improving animal health.
The invention has the following advantages:
The preparation method of glutamate chelate iron provided by the invention has many advantages, such as that easy to operate, the reaction time is short, gained
Iron in product is ferrous iron, is not easy to be oxidized ferric iron, can be used as benefit iron new product in livestock and poultry cultivation and plays its effect, ecology
Environmental security is suitable for producing upper large-scale application.
Detailed description of the invention
Fig. 1 is the X-ray diffractogram of the sample of different irradiation doses in the embodiment of the present invention.
Fig. 2 is the X-ray diffractogram of the sample of different material molar ratio in the embodiment of the present invention.
The X-ray diffractogram of sample when Fig. 3 is different pH value in the embodiment of the present invention.
The X-ray diffractogram of sample when Fig. 4 is differential responses temperature in the embodiment of the present invention.
The X-ray diffractogram of sample when Fig. 5 is the differential responses time in the embodiment of the present invention.
Fig. 6 is Pidolidone and glutamate chelate iron infrared spectrogram.
Specific embodiment
Hereinafter, preferred embodiments of the present invention will be described, it should be understood that preferred embodiment described herein is only used
In the description and interpretation present invention, it is not intended to limit the present invention.
Embodiment 1
Present embodiments provide a kind of preparation method of the preparation method of glutamate chelate iron；Specifically includes the following steps:
1.1 materials and methods
1.1.1 main agents and instrument
Pidolidone (L-Glu), purity 98%, biochemical reagents；Frerrous chloride, purity 99% are analyzed pure；Ethyl alcohol, go from
Sub- water is commercially available.
Electron accelerator, the CAS Institute of Modern Physics；Electronic balance, Mei Tele ME series；DF101S
Thermal-arrest blender, Shanghai Yue Zhong Instrument Ltd.；6700 Fourier transformation infrared spectrometer of Buddhist nun's high-tensile strength, U.S. Buddhist nun high-tensile strength instrument
Company；Thermo Scientific iCETM3000 atomic absorption spectrophotometers, thermoelectricity instrument company, the U.S..
1.1.2 synthesis step
By the glutamic acid (0.068mol) of 10g, 100mL water is dissolved in three-neck flask, and heating water bath is molten to 40 DEG C of constant temperature
The frerrous chloride (0.068mol) of 8.62g is added in Xie Hou, with 40wt% sodium hydroxide solution tune pH to 4, set irradiation temperature as
40 DEG C, which is put into irradiation platform, by electron beam irradiation (electron beam 10MeV), dosage 1.50kGy, irradiation terminates
Afterwards, after controlling reaction time 5min, after reaction, reaction solution is centrifuged 20min in 3000 revolving speeds, supernatant adds the 90vt% of 50mL
Industrial alcohol, place refrigerator overnight, obtain sample pellet, place in 40 DEG C of vacuum desiccators dry 4h, product is placed in close
Seal preservation in sample sack.
The analysis of 1.2 glutamate chelate iron samples
Sample chelation percent is measured using atomic absorption spectrophotometer, passes through infrared spectrometer (IR), X-ray diffractometer
(XRD) sample is analyzed, determines the constituent of sample.
Chelation percent=sample ferrous ions content/raw material ferrous ions content × %
1.3 glutamate chelate iron optimum preparation conditions
1.3.1 influence of the irradiation dose to sample chelation percent
The electron irradiation dosage that chelate Glutamic Acid is chelated with metal iron ion is not fixed, it is to sample chelation percent
It is affected, the dosage of electron beam irradiation is 1.00~3.00kGy.Research shows that when glutamic acid and metallic iron chelation percent are with it
The raising of irradiation dose and increase, the dosage 2.50kGy of irradiation, chelation percent is maximum.It is shown in Table 1.
Influence of 1 irradiation dose of table to sample chelation percent
| The dosage kGy of irradiation | 1.00 | 1.50 | 2.00 | 2.50 | 3.00 |
| Chelation percent % | 74.3 | 78.7 | 87.2 | 89.2 | 88.3 |
1.3.2 feed molar compares the influence of sample chelation percent
The molar ratio of chelate Glutamic Acid and metal iron ion be not it is fixed, it is the coordination by iron ion and ligand
What mode determined, the molar ratio of chelate Glutamic Acid and iron ion can be 1~3: 1.Research shows that when glutamic acid and metal
Iron molar ratio is affected to sample chelation percent, increases with the raising of its molar ratio, and when molar ratio 2: 1, chelation percent is most
Greatly.It is shown in Table 2.
The influence of 2 feed molar of table comparison sample chelation percent
1.3.3 influence of the pH value of reaction system to sample chelation percent
Influence of the pH value for reaction system is very big, the meeting of pH value difference so that the zwitterion number in solution changes,
And then influence the existence form of glutamic acid in the solution.At material molar ratio n (L-Glu): n (FeCl2)=2.0: 1, reaction temperature
When spending 40 DEG C, by changing the pH value of reaction system, after reacting 10min, the chelation percent of sample under different pH condition is obtained.See
Table 3.
Influence of 3 pH value of reaction system of table to sample chelation percent
| PH value | 1.00 | 2.00 | 3.00 | 4.00 | 5.00 | 6.00 |
| Chelation percent % | 80.3 | 83.7 | 87.2 | 89.2 | 82.3 | 81.1 |
1.3.4 influence of the reaction temperature to sample chelation percent
Chelatropic reaction is an exothermic reaction, therefore reaction temperature is also one of its influence factor, it is generally the case that is changed
The temperature of reaction system can accelerate its reaction speed, its reaction is made to reach balance as early as possible.Reaching optimal reaction temperature simultaneously
Afterwards, continue to increase reaction temperature, its balanced sequence can be made for exothermic reaction, by-product or brokenization product may be generated
Structure, influence the purity and yield of product.Therefore after having investigated 3 irradiation dose, material molar ratio and pH value factors, lead to
The temperature for changing reaction system is crossed, obtains the chelation percent of sample under condition of different temperatures.It is shown in Table 4.
Influence of 4 reaction temperature of table to sample chelation percent
| Reaction temperature DEG C | 20.0 | 30.0 | 40.0 | 50.0 | 60.0 |
| Chelation percent % | 80.3 | 87.7 | 89.2 | 86.4 | 82.3 |
1.3.5 influence of the reaction time to sample chelation percent
Reaction time can also have an impact the chelation percent of sample, and reaction reaches optimum efficiency needs one during chelating
Fixed time, reaction time increase may generate side reaction.Test is in material molar ratio n (L-Glu): n (FeCl2)=2.0:
1, pH value of reaction system 4, when temperature is 50 DEG C, by changing the reaction time of system, sample when obtaining the differential responses time
Chelation percent.It is shown in Table 5.
Influence of 5 reaction time of table to sample chelation percent
| Reaction time min | 1.0 | 3.0 | 5.0 | 7.0 | 9.0 |
| Chelation percent % | 80.3 | 88.7 | 89.2 | 82.3 | 77.2 |
The infrared analysis of 1.4 samples
In organic molecule, when with Infrared irradiation organic molecule, chemical bond or functional group in molecule can occur
Absorption of vibrations, since different chemical bonds or functional group's absorption frequency are different, thus they will be in difference on infrared spectroscopy
Position, due to different location, to can get the information of chemical bond or functional group in molecule.
The present invention uses irradiation method to prepare glutamate chelate iron for the first time, and compared with general technology, process flow operation simplifies,
Solvent usage amount is reduced, and by test and phenetic analysis, is obtained best glutamate chelate iron reaction condition, is determined prepared sample
Product are glutamate chelate iron, and maximum chelation percent is 89.2%.
Embodiment 2
Influence of two kinds of iron-supplementing preparations to suckling pig content of hemoglobin and its growth performance
Iron is one of microelement necessary to animal, is a variety of oxidizing ferment such as hemoglobin, myoglobins, cytochromes
Important composition ingredient has close relationship with hematopoietic function, the transport of oxygen, intracellular biological oxidation process and immunity function.
However, piglet seldom has an opportunity to touch the iron in soil under conditions of the closing of modern rearing conditions, intensive.Iron deficiency meeting
Causing piglet that anaemia occurs, shows as skin and mucous membrane is pale, coat is slightly random, appetite stimulator, growth retardation, diarrhea etc.,
Influence the growth performance of piglet.In detection blood the content of hemoglobin cannot illustrate completely piglet whether anaemia, but blood red egg
White content is low can centainly to illustrate piglet anaemia, so can reflect iron-supplementing preparation indirectly by detecting content of hemoglobin
Quality and benefit iron time.
1 material and method
1.1 materials prepare
1.1.1 ferrous gluconate oral solution, Jiangxi east Rong Shiye (group) Co., Ltd produce, iron content in every 10ml
2.68mg；Glutamate chelate iron oral liquid, Lanzhou Livestock and Animal Drug Inst., Chinese Academy of Agricultural Science, iron content in every 10ml
2.68mg。
1.1.2 hemoglobin analyser
Hemoglobin analyser (URIT15) and matched hemoglobin test-paper (H12) are purchased from Guilin Uritest doctor
Treat Electronics Co., Ltd..
1.1.3 experimental animal is grouped
30 piglets are selected, stochastic averagina is divided into two groups, is labeled as 1,2 two group.Wherein use glutamate chelate iron mouth for 1 group
Liquid iron-supplementing preparation is taken, 2 groups use ferrous gluconate oral solution iron-supplementing preparation.
1.2 test method
Every nest piglet cannot be entrusted one's child to the care of sb. during the test, guarantee piglet from birth to off-test in the same feeding management
It is raised under environment, concrete operations such as table 6.
2 test results
Each group birth weight, daily gain and content of hemoglobin data statistics, such as table 7.
Table 6 mends iron
Each index statistical form of table 7
The weight gain of 2.1 piglets is analyzed
As shown in Table 7,1 group of test starting counterpoise is (1.73 ± 0.36) kg；1 group of weaning weight is after the test
(6.94 ± 1.54) kg, net gain (5.21 ± 1.18) kg.Starting counterpoise (1.71 ± 0.30) kg of 2 groups of piglets, examination
Weaning weight is (6.15 ± 1.46) kg after testing, and net gain is (4.44 ± 1.16) kg.It can be seen that being existed using 1 group of pig
Net gain is increased weight 0.77kg more than 2 groups.
The content of hemoglobin of 2.2 piglets is analyzed
As shown in Table 7,1 group of 5 age in days content of hemoglobin of piglet is (79.7 ± 12.94) g/L；10 age in days hemoglobins contain
Amount is (93.0 ± 5.93) g/L；20 age in days content of hemoglobin are (121.6 ± 9.30) g/L.2 groups of 5 age in days hemoglobins of piglet
Content is (79.8 ± 12.32) g/L；10 age in days content of hemoglobin are (86.2 ± 5.79) g/L；20 age in days content of hemoglobin
For (119.6 ± 4.50) g/L.It is lower than 1 group in the content of hemoglobin of 10 and 20 ages in days, 2 groups of piglets.
In conclusion increase weight and content of hemoglobin in terms of 1 group be substantially better than 2 groups.
It is merely a preferred embodiment of the present invention, is not intended to restrict the invention, although referring to aforementioned implementation described in upper
Invention is explained in detail for example, for those skilled in the art, still can be to foregoing embodiments
Documented technical solution is modified or equivalent replacement of some of the technical features.It is all in spirit of the invention
Within principle, any modification, equivalent replacement, improvement and so on be should all be included in the protection scope of the present invention.
Claims (4)
1. a kind of preparation method of glutamate chelate iron, which is characterized in that solution is made in glutamic acid and frerrous chloride, carries out electricity
Beamlet irradiation, separating obtained solid, as glutamate chelate iron.
2. the preparation method of glutamate chelate iron according to claim 1, which is characterized in that the method specifically include as
Lower step:
(1) glutamic acid and frerrous chloride are configured to mixed solution according to molar ratio 1-3:1, after adjusting pH value to 1.0-6.0, into
Row electron beam irradiation 1.0-9.0min, 20-60 DEG C of irradiation temperature, the dosage of electron beam irradiation is 1.00-3.00kGy；
(2) by step (1) irradiation after solution be centrifuged, mixed solvent, be precipitated precipitating, be separated by solid-liquid separation, by obtained solid into
Row it is dry to get.
3. the preparation method of glutamate chelate iron according to claim 2, which is characterized in that in step (1), glutamic acid with
The preferred molar ratio of frerrous chloride is 2:1；
PH value is preferably adjusted to 4, and pH adjusting agent is sodium hydroxide solution；
The electron beam irradiation time is preferably 5min, and irradiation temperature is preferably 40 DEG C, and irradiation dose is preferably 2.50kGy.
4. the preparation method of glutamate chelate iron according to claim 2, which is characterized in that in step (2), solvent is
90vt% ethyl alcohol.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113735729A (en) * | 2021-08-03 | 2021-12-03 | 四川吉隆达生物科技集团有限公司 | Production process of feed-grade ferrous glutamate |
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| CN1566087A (en) * | 2003-06-13 | 2005-01-19 | 吴琼 | Amino acid iron chelate, preparation and application thereof |
| CN1634872A (en) * | 2004-11-02 | 2005-07-06 | 江南大学 | Method for preparing glycine iron(II) chelate for fortified food |
| CN103082089A (en) * | 2011-11-03 | 2013-05-08 | 青岛康地恩药业股份有限公司 | Preparation method of methionine trace element chelate |
| CN109180510A (en) * | 2018-08-29 | 2019-01-11 | 长沙兴嘉生物工程股份有限公司 | A kind of preparation method of high-purity ferrous glutamate |
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2019
- 2019-04-11 CN CN201910288484.7A patent/CN110041213A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1566087A (en) * | 2003-06-13 | 2005-01-19 | 吴琼 | Amino acid iron chelate, preparation and application thereof |
| CN1634872A (en) * | 2004-11-02 | 2005-07-06 | 江南大学 | Method for preparing glycine iron(II) chelate for fortified food |
| CN103082089A (en) * | 2011-11-03 | 2013-05-08 | 青岛康地恩药业股份有限公司 | Preparation method of methionine trace element chelate |
| CN109180510A (en) * | 2018-08-29 | 2019-01-11 | 长沙兴嘉生物工程股份有限公司 | A kind of preparation method of high-purity ferrous glutamate |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113735729A (en) * | 2021-08-03 | 2021-12-03 | 四川吉隆达生物科技集团有限公司 | Production process of feed-grade ferrous glutamate |
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Application publication date: 20190723 |