CN106260602A - A kind of Preparation method and use of strong chelating intensity protein-zinc feed additive - Google Patents
A kind of Preparation method and use of strong chelating intensity protein-zinc feed additive Download PDFInfo
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- CN106260602A CN106260602A CN201610656578.1A CN201610656578A CN106260602A CN 106260602 A CN106260602 A CN 106260602A CN 201610656578 A CN201610656578 A CN 201610656578A CN 106260602 A CN106260602 A CN 106260602A
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Abstract
The present invention relates to the preparation method and application of a kind of strong chelating intensity protein-zinc feed additive, with soybean protein isolate and feed level zinc sulfate as reaction raw materials, soybean separation proteolysis liquid is obtained by hydrolyzed soy separation albumen, fresh water supply system synthetic method makes soybean separation proteolysis liquid and zinc sulfate that chelatropic reaction, preparation strong chelating intensity protein-zinc novel fodder additive to occur under optimum conditions.Present invention also offers strong chelating intensity protein-zinc prepared by described method and be used as the purposes of chicken new zinc source feed additive；Compared with zinc sulfate and conventional organic zinc additive, the product chelating intensity of the present invention is suitable, has higher biological value, it is possible to reduce zinc discharges the environmental pollution caused.The reaction raw materials of the inventive method is cheap and easy to get, and uses current organic trace element main flow synthesis technique aqueous systems synthetic method, has the advantages such as reaction yield high (more than 75%), product chelating intensity favorable reproducibility, simple to operate, cost is relatively low.
Description
Technical field
The present invention relates to the preparation method of a kind of additive of organic zinc feed, specifically, be a kind of strong chelating intensity egg
The Preparation method and use of white zine.
Background technology
Trace element is one of necessary nutritional factors of animal, for solving the deficiency of micronutrient levels in animal feed,
People have done substantial amounts of work in terms of trace mineral supplement.Zinc is one of necessary trace element of animal, has promotion raw
The physiological function that long growth is important with the immune function of body, the integrity safeguarding cell membrane etc., take part in each of vital movement
Individual link, thus it is referred to as " biological element " (Liang Jianguang, 2006).Traditional zinc preparation, such as zinc sulfate and zinc oxide etc., can break
Vitamin in bad feedstuff and other active substances, and animal relatively low to its absorption rate (only 30-60%), do not absorb in a large number
Zinc excrete with feces, both wasted limited mineral element resource, also to environment cause bigger pollution (in sunlight,
2008).Therefore, the Stability Analysis of Structures of new generation developed in recent years, the amino-acid zinc chelate with higher biological activity
And protein-zinc, cause the extensive concern (Luo Xugang, 2004) of people.
Holwerda etc. (1995) close state according to network (chela) compound equilibrium relation and network (chela) and non-network (chela) closes state metal
The half wave potential difference Δ E of ion proposes parameter Q representing that network (chela) closes intensityf, and specify QfBe worth between 1～10 for weak network
(chela) close intensity, between 10～100 for medium network (chela) close intensity, between 100～1000 for strong network (chela) close intensity,
More than 1000 is that extremely strong network (chela) closes intensity.This laboratory on this basis, further improves the network of Organic Manganese, organic zinc
(chela) closes strength detection method, and the biology to milch cow in the absorption in broiler chicken small intestinal of the different shape zinc and organic zinc source
Activity aspect is done a lot of work, and achieves a series of achievement in research.Such as the absorption with ligation perfusion intestinal segment method research zinc in situ
Finding during kinetics model, zinc is a mistake that is saturated and that have carrier to participate in regulation in the absorption of broiler duodenum and jejunum
Journey, is then unsaturation diffusion process in ileum；The absorbance of organic zinc is higher than inorganic zinc, and absorbance chelates intensity with it
Having a close relationship, and the organic zinc chelating by force intensity with polar biased absorbs best, medium chelating intensity is taken second place, and weak chelating intensity is
Secondary (in sunlight, 2008；Yu etc., 2008,2010).Different chelating intensity organic zinc sources, chelating intensity organic zinc source the most by force,
Can avoid to some extent in digestive tract high phytic acid to its absorption or (with) precipitation and the (Huang Yan that is absorbed and used more
The tinkling of pieces of jade, 2007).Organic zinc source stability in cud is better than zinc sulfate source, wherein with strong chelating intensity organic zinc source for
Good, the rumen bypass rate of medium chelating intensity organic zinc source and zinc dissolubility are all minimum (Liang Jianguang, 2006).
Above series achievement in research recently all shows, the chelating intensity of organic zinc be affect that it absorbs main because of
Element.Therefore, research and development product yield is high and the strong of chelating intensity favorable reproducibility chelates intensity organic zinc production technology, for subtracting
The blindness of few organic zinc source produces adds with poor efficiency, reduces environmental pollution, is respectively provided with important theory and realistic meaning.
The synthetic method of current Chelates of Amino Acids And Trace Elements mainly has two kinds, is that liquid phase synthesis produces and solid phase respectively
Synthetically produced (Zhang Feng, 2008).Liquid phase synthesizing method includes aqueous systems synthetic method and non-aqueous system synthetic method, refer to by aminoacid with
Soluble metallic salt is dissolved in water in the organic solvents such as (aqueous systems synthetic method) or ethanol (non-aqueous system synthetic method), suitably adjusts
After joint pH, there is chelatropic reaction in a heated condition, scrubbed, prepare product after drying.Solid-phase synthesis includes solid phase microwave
Method and solid phase room temperature method.After solid phase microwave method refers to mix slaine with aminoacid, add a small amount of water, close after microwave catalysis
Become；Solid phase room temperature method refers to, by after aminoacid and slaine mixed grinding, be dried and i.e. prepare product after the two fully reacts.Gu
Phase synthesi is easy and simple to handle to save time, but needs constantly to be ground reactant mixing in course of reaction, reduces combined coefficient,
Thus be difficult to obtain target product.Liquid phase synthesizing method is the most ripe on reaction condition and technology, and generally can obtain higher
Chelation percent, thus become current organic trace element produce main flow synthesis technique (punishment grain husk, 2011；Wang Lixia, 2013).Closely
Nian Laiyong liquid phase synthesizing method inquire into organic trace element synthesis condition have been reported that more (Kong Suifei, 2011；Force is built just etc., and 2008；
Zhong Guoqing, 2011；Shu Xu is firm, and 2014；Guan Haiyue etc., 2008；Zhang Ruihua, 2004), but produce strong chelating with liquid phase synthesizing method
Intensity organic zinc, then be not reported in the domestic and foreign literature found so far.
Summary of the invention
First purpose of the present invention is to provide the preparation method of a kind of strong chelating intensity protein-zinc, and product chelating intensity is fitted
Preferably, chelating intensity level is all between 100～1000.
Second object of the present invention, is to provide strong chelating intensity protein-zinc made above and is used as chicken new zinc source feedstuff
The purposes of additive, i.e. presses aforesaid operations flow process preparation strong chelating intensity protein-zinc, by addition to mix homogeneously in chicken feed
The most feeding, thus promote that zinc is absorbed by chicken body, it is possible to reduce zinc discharges the environmental pollution caused.
The technology of the present invention solution: the preparation method of a kind of strong chelating intensity protein-zinc feed additive, divides with Semen sojae atricolor
It is reaction raw materials from albumen and feed level zinc sulfate, obtains soybean separation proteolysis liquid by hydrolyzed soy separation albumen, use
Aqueous systems synthetic method makes soybean separation proteolysis liquid and zinc sulfate generation chelatropic reaction, and reaction condition is: (1) soybean separation protein
White and zinc sulfate mass ratio is 4:1 or 6:1, pH value is 7, temperature 60 C and response time 30min, or (2) soybean protein isolate
With zinc sulfate mass ratio be 2:1, pH value be 5, temperature 60 C and response time 30min, or (3) soybean protein isolate and zinc sulfate
Mass ratio is 2:1, pH value is 7, temperature 60 C and response time 120min, and reactant liquor is concentrated to give after reaction a large amount of precipitation,
By 90% washing with alcohol precipitation multipass (such as 3 times etc.), crushed after being dried after Li Xin, prepare strong chelating intensity protein-zinc and produce
Product.
The Q of described strong chelating intensityfMeasured value is 100 to 1000.
Wherein hydrolyzed soy separation protein requirement soybean separation proteolysis specific enzyme；Described specific enzyme is a kind of compounding
Protease includes restriction endonuclease, peptide ending enzyme and food flavor enzyme, various vegetable proteins can be hydrolyzed into peptone, polypeptide and aminoacid.
The technological process of described hydrolyzed soy separation albumen is: weigh soybean protein isolate in beaker, adds ultra-pure water
Concentration of substrate is adjusted to 15%, adds the soybean separation proteolysis specific enzyme of substrate weight 1%, use 40% sodium hydroxide solution
Regulation soybean protein isolate solution ph is 7.5～8.0, is warming up to 85 under the conditions of 54～56 DEG C after continuous stirring hydrolysis 10h
DEG C enzyme denaturing 10min, is filtrated to get soybean separation proteolysis liquid.
Wherein precipitation uses centrifugation, and process is 3000～4000r/min to be centrifuged 5～15min under room temperature.
Wherein reactant liquor concentration process can be decompression rotary evaporation, spray drying, vacuum lyophilization or baking oven hot blast
It is dried；Described baking temperature is 60～80 DEG C.
Wherein the reagent of regulation pH value used is 40% sodium hydroxide solution.
Beneficial effects of the present invention:
(1) the strong preparation method chelating intensity protein-zinc novel fodder additive of the present invention, by this method operation preparation
The product obtained is and chelates by force intensity, it is achieved thereby that by the chelating intensity adjusting reaction process condition regulation and control product, right
It is respectively provided with fabulous answering with poor efficiency interpolation, raising Production of Livestock and Poultry benefit, minimizing environmental pollution etc. in reduction organic zinc blindness production
Use prospect.
(2) reaction raw materials that the present invention not only selects is cheap and easy to get, and uses current organic trace element to produce main flow
Synthesis technique～aqueous systems synthetic method, the most mature and stable, reaction yield is up to more than 75%, synthesizes with low cost, has
Fabulous popularizing application prospect.
Detailed description of the invention
The key step of the inventive method: weigh reaction raw materials soybean protein isolate → hydrolyzed soy separation albumen and obtain big
Bean separation proteolysis liquid → weighing feed level zinc sulfate → in aqueous medium, in the case of dissolving → heated and stirred, Semen sojae atricolor separates
Separate out after protein hydrolyzate and zinc sulfate generation chelatropic reaction → reactant liquor are concentrated precipitation → under 3000～4000r/min from
The heart 5～the 3 times → dry → pulverizing of 90% washing with alcohol of 15min → abandoning supernatant → precipitation prepare strong chelating intensity egg
White zine novel fodder additive.
During chelatropic reaction, the technological parameter condition of reaction can be set as following three kinds: (1) soybean protein isolate
With zinc sulfate mass ratio be 4:1 or 6:1, pH value be 7, temperature 60 C and response time 30min；(2) soybean protein isolate and sulfur
Acid zinc mass ratio is 2:1, pH value is 5, temperature 60 C and response time 30min；(3) soybean protein isolate and zinc sulfate mass ratio
For 2:1, pH value be 7, temperature 60 C and response time 120min.The protein-zinc prepared under these conditions is strong chelating intensity egg
White zine.
Reactant liquor condensing mode includes reduce pressure rotary evaporation, lyophilisation, baking oven hot air drying or spray drying；Institute
Stating baking temperature is 60～80 DEG C.
Course of reaction needs with 40% sodium hydroxide solution regulation pH value.
The present invention is discussed in detail below in conjunction with specific embodiment.But below example is only limitted to explain the present invention, this
Bright protection domain should include the full content of claim, is not limited only to the present embodiment.
Embodiment 1
Weighing 70g soybean protein isolate, adding ultra-pure water regulation concentration of substrate is 15%, adds the big of substrate weight 1%
Bean separation proteolysis specific enzyme, is 8.0 by 40% sodium hydroxide solution regulation soybean protein isolate solution ph, in 55 DEG C of bars
It is warming up to 85 DEG C of enzyme denaturing 10min after continuous stirring hydrolysis 10h under part, is filtrated to get soybean separation proteolysis liquid.Former by reaction
Material soybean protein isolate weighs 35g feed level zinc sulfate with zinc sulfate mass ratio 2:1, is dissolved in ultra-pure water by zinc sulfate, extremely
After being completely dissolved, being mixed with solution of zinc sulfate by soybean separation proteolysis liquid, stirring is warming up to 60 DEG C and keeps temperature constant,
It is 5 with 40% sodium hydroxide solution regulation reacting liquid pH value, after reaction 30min, places reaction liquid into hot blast in baking oven and be concentrated into
Crystalline film occurs, cools down at room temperature after taking out from baking oven, separates out a large amount of precipitation.4000r/min is centrifuged 10min, discards
Clear liquid, precipitation is placed in 75 DEG C of baking ovens drying for three times with 90% ethanol wash, crosses 40 mesh sieves, preserve after packaging after pulverizing.Produce
Product yield is 87%；Obtaining sample zinc content with Atomic Absorption Spectrometry is 11.1%；Sample chelating intensity is recorded by polarography
It is 137.
Embodiment 2
Weighing 70g soybean protein isolate, adding ultra-pure water regulation concentration of substrate is 15%, adds the big of substrate weight 1%
Bean separation proteolysis specific enzyme, is 8.0 by 40% sodium hydroxide solution regulation soybean protein isolate solution ph, in 55 DEG C of bars
It is warming up to 85 DEG C of enzyme denaturing 10min after continuous stirring hydrolysis 10h under part, is filtrated to get soybean separation proteolysis liquid.Former by reaction
Material soybean protein isolate is that 2:1 weighs 35g zinc sulfate with zinc sulfate mass ratio, is dissolved in ultra-pure water by zinc sulfate, to completely
After dissolving, being mixed with solution of zinc sulfate by soybean separation proteolysis liquid, stirring is warming up to 60 DEG C and keeps temperature constant, uses
40% sodium hydroxide solution regulation reacting liquid pH value is 7, after reaction 120min, places reaction liquid into hot blast in baking oven and is concentrated into knot
Epitaxial occurs, cools down at room temperature after taking out from baking oven, separates out a large amount of precipitation.4000r/min is centrifuged 10min, supernatant discarded
Liquid, precipitation is washed continuously three times with 90% ethanol and is placed in 75 DEG C of baking ovens drying, crosses 40 mesh sieves, preserve after packaging after pulverizing.
Product yield is 83.6%；Obtaining sample zinc content with Atomic Absorption Spectrometry is 10.2%；Sample chelating is recorded by polarography
Intensity is 199.
Embodiment 3
Weighing 70g soybean protein isolate, adding ultra-pure water regulation concentration of substrate is 15%, adds the big of substrate weight 1%
Bean separation proteolysis specific enzyme, is warming up to 85 DEG C of enzyme denaturing 10min after continuous stirring hydrolysis 10h under the conditions of 55 DEG C, filters
To soybean separation proteolysis liquid.It is that 4:1 weighs 17.5g sulphuric acid by reaction raw materials soybean protein isolate and zinc sulfate mass ratio
Zinc, is dissolved in zinc sulfate in ultra-pure water, after being completely dissolved, is mixed with solution of zinc sulfate by soybean separation proteolysis liquid,
Stirring is warming up to 60 DEG C and keeps temperature constant, is 7 with 40% sodium hydroxide solution regulation reacting liquid pH value, after reaction 30min,
Placing reaction liquid into hot blast in baking oven and be concentrated into crystalline film appearance, cool down at room temperature after taking out from baking oven, it is a large amount of heavy to separate out
Form sediment.4000r/min is centrifuged 10min, abandoning supernatant, and precipitation is washed continuously three times with 90% ethanol and is placed in 75 DEG C of baking ovens baking
Dry, cross 40 mesh sieves after pulverizing, preserve after packaging.Product yield is 86.5%；Sample zinc content is obtained with Atomic Absorption Spectrometry
It is 6.52%；Recording sample chelating intensity by polarography is 757.
Embodiment 4
Weighing 70g soybean protein isolate, adding ultra-pure water regulation concentration of substrate is 15%, adds the big of substrate weight 1%
Bean separation proteolysis specific enzyme, is warming up to 85 DEG C of enzyme denaturing 10min after continuous stirring hydrolysis 10h under the conditions of 55 DEG C, filters
To soybean separation proteolysis liquid.It is that 6:1 weighs 11.67g sulphuric acid by reaction raw materials soybean protein isolate and zinc sulfate mass ratio
Zinc, is dissolved in zinc sulfate in ultra-pure water, after being completely dissolved, is mixed with solution of zinc sulfate by soybean separation proteolysis liquid,
Stirring is warming up to 60 DEG C and keeps temperature constant, is 7 with 40% sodium hydroxide solution regulation reacting liquid pH value, after reaction 30min,
Placing reaction liquid into hot blast in baking oven and be concentrated into crystalline film appearance, cool down at room temperature after taking out from baking oven, it is a large amount of heavy to separate out
Form sediment.4000r/min is centrifuged 10min, abandoning supernatant, and precipitation is washed continuously three times with 90% ethanol and is placed in 75 DEG C of baking ovens baking
Dry, cross 40 mesh sieves after pulverizing, preserve after packaging.Product yield is 76.5%；Sample zinc content is obtained with Atomic Absorption Spectrometry
It is 4.22%；Recording sample chelating intensity by polarography is 193.
In a word, the product chelating intensity of the present invention is suitable, has higher biological value, can more effectively prevent and treat chicken
Deng poultry zinc deficiency, reduce zinc and discharge the environmental pollution caused.The reaction raw materials of the inventive method is cheap and easy to get, and uses current
Organic trace element main flow synthesis technique aqueous systems synthetic method, has reaction yield high (more than 75%), product chelating intensity weight
The existing advantages such as property is good, simple to operate, cost is relatively low.
It should be noted that according to the various embodiments described above of the present invention, those skilled in the art are to realize this completely
The four corner of bright independent claims and appurtenance, it is achieved process and the same the various embodiments described above of method；And the present invention is not
Elaborate and partly belong to techniques well known.
The above, part detailed description of the invention the most of the present invention, but protection scope of the present invention is not limited thereto, and appoints
How those skilled in the art are in the technical scope that the invention discloses, the change that can readily occur in or replacement all should be contained
Within protection scope of the present invention.
Claims (9)
1. the preparation method of one kind strong chelating intensity protein-zinc feed additives, it is characterised in that: with soybean protein isolate and feedstuff
Level zinc sulfate is reaction raw materials, obtains soybean separation proteolysis liquid, fresh water supply system synthetic method by hydrolyzed soy separation albumen
Making soybean separation proteolysis liquid and zinc sulfate generation chelatropic reaction, reaction condition is: (1) soybean protein isolate and zinc sulfate matter
Amount than is 4:1 or 6:1, pH value be 7, temperature 60 C and response time 30min, or (2) soybean protein isolate and zinc sulfate quality
Than be 2:1, pH value be 5, temperature 60 C and response time 30min, or (3) soybean protein isolate and zinc sulfate mass ratio be 2:1,
PH value is 7, temperature 60 C and response time 120min, reactant liquor is concentrated to give after reaction a large amount of precipitation, washing precipitation, is dried
Rear pulverizing, prepares strong chelating intensity protein-zinc product；The Q of described strong chelating intensityfMeasured value is 100 to 1000.
The preparation method of strong chelating intensity protein-zinc feed additive the most according to claim 1, it is characterised in that: wherein
Hydrolyzed soy separation protein requirement soybean separation proteolysis specific enzyme；In described specific enzyme includes for the compounding protease of one
Cut enzyme, peptide ending enzyme and food flavor enzyme, various vegetable proteins can be hydrolyzed into peptone, polypeptide and aminoacid.
The preparation method of strong chelating intensity protein-zinc feed additive the most according to claim 1, it is characterised in that: described
The technological process of hydrolyzed soy separation albumen is: weigh soybean protein isolate in beaker, adds ultra-pure water and is adjusted by concentration of substrate
It is 15%, adds the soybean separation proteolysis specific enzyme of substrate weight 1%, separate with 40% sodium hydroxide solution regulation Semen sojae atricolor
Protein solution pH value is 7.5～8.0, is warming up to 85 DEG C of enzyme denaturing 10min under the conditions of 54～56 DEG C after continuous stirring hydrolysis 10h,
It is filtrated to get soybean separation proteolysis liquid.
The preparation method of strong chelating intensity protein-zinc feed additive the most according to claim 1, it is characterised in that: wherein
Precipitation uses centrifugation, and process is 3000～4000r/min to be centrifuged 5～15min under room temperature.
The preparation method of strong chelating intensity protein-zinc feed additive the most according to claim 1, it is characterised in that: wherein
Reactant liquor concentration process can be decompression rotary evaporation, spray drying, vacuum lyophilization or baking oven hot air drying；Described dry
Temperature is 60～80 DEG C.
The preparation method of strong chelating intensity protein-zinc feed additive the most according to claim 1, it is characterised in that: wherein
The reagent of regulation pH value used is 40% sodium hydroxide solution.
The preparation method of strong chelating intensity protein-zinc feed additive the most according to claim 1, it is characterised in that: reaction
After reactant liquor is concentrated to give a large amount of precipitation, precipitate multipass by 90% washing with alcohol.
8., according to the strong chelating intensity protein-zinc feed additive prepared by claim 1～7 one of arbitrarily described method, use
Make the purposes of chicken new zinc source feed additive.
9. according to the purposes of 8 described in claim, wherein using described strong chelating intensity protein-zinc as chicken new zinc source feedstuff
Additive, feeds by addition to after mix homogeneously in chicken feed, thus promotes the chicken absorption to zinc.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2021147361A1 (en) * | 2020-01-22 | 2021-07-29 | 广州大学 | Zinc ion complex peptide, and complex and use thereof |
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2016
- 2016-08-11 CN CN201610656578.1A patent/CN106260602A/en active Pending
Non-Patent Citations (1)
| Title |
|---|
| 高素蕴: "大豆多肽锌螯合盐的制备及生理活性研究", 《中国优秀博硕士学位论文全文数据库 (硕士)工程科技Ⅰ辑》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2021147361A1 (en) * | 2020-01-22 | 2021-07-29 | 广州大学 | Zinc ion complex peptide, and complex and use thereof |
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Application publication date: 20170104 |