CN109430560A - A kind of zinc oxide feed addictive and its preparation method and application - Google Patents
A kind of zinc oxide feed addictive and its preparation method and application Download PDFInfo
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- CN109430560A CN109430560A CN201811593241.6A CN201811593241A CN109430560A CN 109430560 A CN109430560 A CN 109430560A CN 201811593241 A CN201811593241 A CN 201811593241A CN 109430560 A CN109430560 A CN 109430560A
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- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23K—FODDER
- A23K50/00—Feeding-stuffs specially adapted for particular animals
- A23K50/30—Feeding-stuffs specially adapted for particular animals for swines
-
- 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
- A23K20/105—Aliphatic or alicyclic compounds
-
- 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
- A23K20/116—Heterocyclic compounds
- A23K20/121—Heterocyclic compounds containing oxygen or sulfur as hetero atom
-
- 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
- A23K20/116—Heterocyclic compounds
- A23K20/137—Heterocyclic compounds containing two hetero atoms, of which at least one is nitrogen
-
- 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
- A23K20/158—Fatty acids; Fats; Products containing oils or fats
-
- 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
- A23K20/20—Inorganic substances, e.g. oligoelements
- A23K20/30—Oligoelements
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23K—FODDER
- A23K50/00—Feeding-stuffs specially adapted for particular animals
- A23K50/60—Feeding-stuffs specially adapted for particular animals for weanlings
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K33/00—Medicinal preparations containing inorganic active ingredients
- A61K33/24—Heavy metals; Compounds thereof
- A61K33/30—Zinc; Compounds thereof
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61P—SPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
- A61P1/00—Drugs for disorders of the alimentary tract or the digestive system
- A61P1/12—Antidiarrhoeals
Abstract
The present invention relates to a kind of zinc oxide feed addictives and its preparation method and application, belong to field of feed additive technology, the additive by mass percentage, including hydrophobicity capsule material 24-58%, hydrophily capsule material 5-15%, zinc oxide 30-70%.This method inlays inclusion technique using hydrophobicity capsule material molecular state and hydrophily capsule material punches disintegration technology, hydrophobicity capsule material in additive, the amount of hydrophily capsule material and zinc oxide three are controlled simultaneously, be destroyed the zinc oxide in the zinc oxide feed addictive finally prepared will not when crossing stomach, reduce the disintegration dissolution of zinc oxide under one's belt, keep the molecular state of zinc oxide, and dissolution and major part can be disintegrated with the presence of zinc oxide molecules state in enteron aisle after so that Zinc oxide particles is crossed stomach, to play its enteron aisle convergence anti-CaM antibody.The Additive Production simple process, process is few, and production energy consumption is low, of large quantities, and single batch of yield is suitble to industrialized production up to 2t/h up to 1.0-1.5t, production efficiency.
Description
Technical field
The invention belongs to field of feed additive technology, and in particular to a kind of zinc oxide feed addictive and preparation method thereof
And application.
Background technique
1989, the Foulum National Animal academy of sciences, Denmark was the study found that add 2500- in early-weaned piglets daily ration
4000mg/kg zinc can significantly reduce the diarrhea rate of piglet, and hereafter, numerous studies and production practices prove, adding high zinc not only has
Effect, it is also very economical.Agricultural University Of He'nan's Wang Zhixiang paper " discussion of zinc oxide anti diar rhea mechanism " report, zinc oxide anti diar rhea
Mechanism can be divided into three categories: 1. zinc oxide can improve Intestinal Morphology and digestive system functions, avoid indigestion
Caused diarrhea；2. zinc oxide has certain fungistatic effect, the risk that pathogen invasion causes pathologic diarrhea can be reduced；③
The expression of a variety of factors of the adjustable immune system of zinc oxide, avoids allergic diarrhea while providing immunoprotection for body.
Most literature thinks that zinc oxide anti diar rhea worked is zinc oxide molecules state, rather than zinc ion, so must avoid aoxidizing
Decomposition of the zinc in gastric acid environment.
The feed addictive Method of ZnO to circulate currently on the market will have: common zinc oxide, Nano-class zinc oxide, porous type
Zinc oxide, enteric coated zinc oxide etc..These types of zinc oxide all haves the defects that different, and first three zinc oxide simulates stomach in vitro
Dissolution is more than 90%, i.e., most of to enter enteron aisle with Zinc ion form, wherein nanoscale oxygen in liquid (pH=1.2 and pH=4.3)
Changing zinc, there is also reunions, and bulk density is low, is not easy the disadvantages of being uniformly mixed with feed.Although enteric coated zinc oxide can guarantee stomach,
But traditional mixing, granulation, the coated production technology of fluidized bed are all used, it is long that there are process flows, and energy consumption is high, and production efficiency is low
The disadvantages of, and coating material need to be dissolved with inflammable organic solvent, there are some potential safety problemss.Also, with becoming for regulation
Sternly, the decrement trend in feed of zinc oxide is obvious.Therefore, by preparation technique, a kind of novel, efficient mixed type is developed
Zinc oxide feed addictive is very necessary.
Summary of the invention
In view of this, one of the objects of the present invention is to provide a kind of zinc oxide feed addictives；The second purpose is to mention
For a kind of preparation method of zinc oxide feed addictive；The third purpose is to provide zinc oxide feed addictive in preparing feed
Application.
In order to achieve the above objectives, the invention provides the following technical scheme:
1, a kind of zinc oxide feed addictive, by mass percentage, the additive include following group and are grouped as: hydrophobic
Property capsule material 24-58%, hydrophily capsule material 5-15%, zinc oxide 30-70%.
Preferably, the hydrophobicity capsule material is at least one of monoglyceride, hydrogenated oil and fat, paraffin, palm oil or peanut oil.
Preferably, the hydrophily capsule material is in PEG1000, PEG1500, PEG4000, PEG6000 or poloxamer
It is at least one.
2, the preparation method of a kind of zinc oxide feed addictive, the method specifically: by hydrophobicity capsule material and
Hydrophily capsule material mixes after being respectively melted, and zinc oxide is then added, and obtains mixture after mixing again, the mixture is carried out
Spray chilling.
Preferably, the temperature of the fusing is 100-130 DEG C.
Preferably, zinc oxide is added at 80-90 DEG C.
Preferably, the spray chilling specifically: the mixture is sent to centrifugal spray tower, the centrifugal spray is controlled
Inlet air temperature≤5 DEG C of tower, centrifugal turntable speed are 3000-4000r/min, air quantity 30000-40000m3/min。
Preferably, zinc oxide feed addictive obtained is sieved after the spray chilling, obtaining particle diameter is
The zinc oxide feed addictive of 40-80 mesh.
3, a kind of zinc oxide feed addictive is preparing the application in feed.
The beneficial effects of the present invention are: the present invention provides a kind of zinc oxide feed addictive and preparation method thereof and answer
With this method inlays inclusion technique using hydrophobicity capsule material molecular state and hydrophily capsule material punches disintegration technology, while control adds
Add hydrophobicity capsule material in agent, the amount of hydrophily capsule material and zinc oxide three, makes in the zinc oxide feed addictive finally prepared
Zinc oxide will not be destroyed when crossing stomach, reduced the disintegration dissolution of zinc oxide under one's belt, kept the molecular state of zinc oxide, and make oxygen
Dissolution and major part can be disintegrated in enteron aisle with the presence of zinc oxide molecules state by changing after zinc particle crosses stomach, to play the convergence of its enteron aisle
Anti-CaM antibody, wherein zinc oxide slowly dissolves out (4.5h) in small intestine leading portion, persistently dissolves out (4.5h-5.5h) in the ileum stage.
In addition, making the weight of zinc oxide feed addictive finally prepared by the process conditions of control spray chilling during the preparation process
In 0.7-0.9kg/L, it is allowed to close with feed bulk density, it is easier to be uniformly mixed with feed.Of the zinc oxide feed addictive
Grain diameter is 40-80 mesh, and is lower than 10% by the ratios of 80 mesh, so that mixed material feeding not dust, to environment and operation fellow worker
It is good.The Additive Production simple process, process is few, and production energy consumption is low, of large quantities, and single batch of yield is up to 1.0-1.5t, production effect
Rate is suitble to industrialized production up to 2t/h.
Detailed description of the invention
In order to keep the purpose of the present invention, technical scheme and beneficial effects clearer, the present invention provides following attached drawing and carries out
Illustrate:
Fig. 1 is preceding 7 days diarrhea rate columns in embodiment 10；
Fig. 2 is rear 7 days diarrhea rate columns in embodiment 10；
Fig. 3 is whole diarrhea rate column in embodiment 10.
Specific embodiment
Below by a preferred embodiment of the present invention will be described in detail.
Reagent used in embodiment is as follows:
In-vitro simulated gastric juice I, the i.e. hydrochloric acid solution of pH=1.2, it is accurate to measure 0.2mol/L hydrochloric acid solution 425mL, add water
Be diluted to 1000mL, shake up to get；
In-vitro simulated gastric juice II, the i.e. acetate buffer solution of pH=4.3 accurately weigh sodium acetate 1.99g and are placed in 1000mL appearance
In measuring bottle, after being dissolved in water be added 2mol/L acetum 17.7mL, dilute and be settled to scale, shake up to get；
In-vitro simulated intestinal juice, the i.e. phosphate buffer of pH=6.8 are accurate to measure 0.2mol/L potassium dihydrogen phosphate test solution
250mL and 0.2mol/L sodium hydroxide solution 112mL is placed in 1000mL volumetric flask, is diluted with water and is settled to scale, shake up,
To obtain the final product；
Dilute hydrochloric acid: it is accurate to measure hydrochloric acid 234mL, be diluted with water to 1000mL, shake up to get.
Embodiment 1
Test hydrophobicity capsule material and hydrophily capsule material respectively with the zinc oxide feed addictive of zinc oxide preparation mould in vitro
Dissolution rate in quasi- gastric juice
By hydrophobicity capsule material and hydrophily capsule material prepared respectively with zinc oxide zinc oxide content be respectively 30wt%,
Then each zinc oxide feed addictive is distinguished mould in vitro by the zinc oxide feed addictive of 40wt%, 50wt% and 70tw%
Intend gastric juice I, tests its dissolution rate in in-vitro simulated gastric juice II.Tested as follows:
Accurately weighed 2g zinc oxide feed addictive sample, is placed in stripping rotor, and using blade method, blade is as far as possible close to molten
Bottom of a cup portion (since oxidation zinc weight proportion is big, and being easy to reunite, sample is prevented to be deposited on bottom of a cup portion) out, adds the in-vitro simulated stomach of 400mL
Liquid, at 37 DEG C after the rotational speed 120min with 100r/min, the accurate 100mL dilute hydrochloric acid that is added is not (because zinc oxide dissolves in
Water, simulate the gastric juice and simulated intestinal fluid etc., but it is dissolved in dilute hydrochloric acid, it is to digest and be released to simulate the gastric juice that dilute hydrochloric acid, which is added,
Or the zinc oxide in simulated intestinal fluid solves homogeneously in simulate the gastric juice or simulated intestinal fluid, is convenient for sample detection), continue with 100r/
It takes solution appropriate after the rotational speed 20min of min, filters, precision measures above-mentioned subsequent filtrate 25.00mL, is placed in 250mL conical flask
In, by HG/T 2792-2011, is titrated and calculated, test result is shown in Table 1.
The in-vitro simulated gastric juice dissolution rate test result of zinc oxide feed addictive made of the different capsule materials of table 1
Note: the mass ratio of palm oil, monoglyceride and hydrogenated oil and fat three is 150:201:134；Peanut oil, monoglyceride and hydrogenation
The mass ratio of oily three is 160:122:82.
It as shown in Table 1, is the zinc oxide in zinc oxide feed addictive prepared by raw material in simulation stomach using hydrophobicity capsule material
It is not easy to be dissolved in liquid, and is the zinc oxide in zinc oxide feed addictive prepared by raw material in simulation stomach using hydrophily capsule material
Dissolution rate has been above 80% in liquid.
Embodiment 2
Using monoglyceride, hydrogenated oil and fat, PEG4000 and zinc oxide as raw material, zinc oxide feed addictive, prepared oxygen are prepared
Change zinc feed additive in monoglyceride, hydrogenated oil and fat, PEG4000 mass percent be shown in Table 2, with zinc oxide feed addictive in body
Dissolution rate in outer simulate the gastric juice and in-vitro simulated intestinal juice is inspection target, carries out three factors, three horizontal orthogonal tests.Its
In, dissolution rate of each zinc oxide feed addictive in vitro in simulate the gastric juice is tested referring to method in embodiment 1, test knot
Fruit is shown in Table 2- table 5；Dissolution rate of each zinc oxide feed addictive in vitro in simulated intestinal fluid is tested as follows:
Accurately weighed 2g zinc oxide feed addictive sample, is placed in stripping rotor, and using blade method, blade is as far as possible close to molten
Bottom of a cup portion (since oxidation zinc weight proportion is big, and being easy to reunite, sample is prevented to be deposited on bottom of a cup portion) out, adds the in-vitro simulated intestines of 400mL
Liquid, at 37 DEG C after the rotational speed 7h with 100r/min, the accurate 100mL dilute hydrochloric acid that is added is (because zinc oxide is not soluble in water, mould
Quasi- gastric juice and simulated intestinal fluid etc., but it is dissolved in dilute hydrochloric acid, it is to digest and be released to simulate the gastric juice or mould that dilute hydrochloric acid, which is added,
Zinc oxide in quasi- intestinal juice solves homogeneously in simulate the gastric juice or simulated intestinal fluid, is convenient for sample detection), continue with 100r/min's
It takes solution appropriate after rotational speed 20min, filters, precision measures above-mentioned subsequent filtrate 25.00mL, is placed in 250mL conical flask, presses
HG/T 2792-2011 is titrated and is calculated, and test result is shown in Table 2- table 5.
2 positive quadraturing design test result of table
The THE PRINCIPAL FACTOR ANALYSIS of 3 monoglyceride of table
The THE PRINCIPAL FACTOR ANALYSIS of 4 hydrogenated oil and fat of table
The THE PRINCIPAL FACTOR ANALYSIS of 5 PEG4000 of table
By table 2 to table 5 it is found that the dissolution rate of zinc oxide increases with the ratio of hydrophobicity capsule material in zinc oxide feed addictive
And decline, increase with the ratio of hydrophily capsule material and increase, according to experimental result, monoglyceride mass fraction is 30%, hydrogenated oil and fat
Zinc oxide dissolution rate is minimum in in-vitro simulated gastric juice when being 25% for mass fraction, but zinc oxide dissolution rate in simulated intestinal fluid in vitro
Also minimum, since the HLB value of hydrogenated oil and fat is greater than monoglyceride, so monoglyceride mass fraction is set as 30%, hydrogenate oil quality
Score is set as 20%.Though PEG4000 can dramatically increase in zinc oxide feed addictive zinc oxide in vitro in simulated intestinal fluid
Dissolution, but the dissolution influence of zinc oxide is also larger in simulate the gastric juice in vitro, therefore the mass fraction of PEG4000 is set as
10%.
Embodiment 3
Prepare zinc oxide feed addictive
By 855kg hydrophobicity capsule material (513kg monoglyceride and 342kg paraffin), 171kg hydrophily capsule material (PEG1500) point
It Tou Ru not be melted in collet heating tank, controlling jacket temperature processed is 100 DEG C, by the hydrophobicity capsule material and hydrophily capsule material after fusing
It is transferred in collet stirring homogeneous tank, maintaining the jacket temperature of stirring homogeneous tank is 80 DEG C, starts blender, is added simultaneously
474kg crude zinc oxide materials (zinc oxide content 95wt%), start Homogenizing pump after mixing evenly, are uniformly mixed material, obtain
Then mixture send the mixture to centrifugal spray tower, control inlet air temperature≤5 DEG C of the centrifugal spray tower, and centrifugation turns
Disk speed is 3000r/min, air quantity 30000m2/ min obtains zinc oxide feed addictive particle, finally using concussion sieve sieve
Point, the zinc oxide feed addictive that particle diameter is 40-80 mesh is collected, metering, is put in storage at packaging after the assay was approved.
Embodiment 4
Prepare zinc oxide feed addictive
By 724kg hydrophobicity capsule material (436kg monoglyceride and 288kg hydrogenated oil and fat), 144kg hydrophily capsule material (PEG4000)
It puts into collet heating tank and melts respectively, controlling jacket temperature processed is 120 DEG C, by the hydrophobicity capsule material and hydrophily capsule after fusing
Material is transferred in collet stirring homogeneous tank, and maintaining the jacket temperature of stirring homogeneous tank is 85 DEG C, is started blender, is added simultaneously
632kg crude zinc oxide materials (zinc oxide content 95wt%), start Homogenizing pump after mixing evenly, are uniformly mixed material, obtain
Then mixture send the mixture to centrifugal spray tower, control inlet air temperature≤5 DEG C of the centrifugal spray tower, and centrifugation turns
Disk speed is 3500r/min, air quantity 32000m2/ min obtains zinc oxide feed addictive particle, finally using concussion sieve sieve
Point, the zinc oxide feed addictive that particle diameter is 40-80 mesh is collected, metering, is put in storage at packaging after the assay was approved.
Embodiment 5
Prepare zinc oxide feed addictive
By 592kg hydrophobicity capsule material (356kg monoglyceride and 236kg hydrogenated oil and fat), 118kg hydrophily capsule material (PEG6000)
It puts into collet heating tank and melts respectively, controlling jacket temperature processed is 115 DEG C, by the hydrophobicity capsule material and hydrophily capsule after fusing
Material is transferred in collet stirring homogeneous tank, and maintaining the jacket temperature of stirring homogeneous tank is 80 DEG C, is started blender, is added simultaneously
790kg crude zinc oxide materials (zinc oxide content 95wt%), start Homogenizing pump after mixing evenly, are uniformly mixed material, obtain
Then mixture send the mixture to centrifugal spray tower, control inlet air temperature≤5 DEG C of the centrifugal spray tower, and centrifugation turns
Disk speed is 3200r/min, air quantity 36000m2/ min obtains zinc oxide feed addictive particle, finally using concussion sieve sieve
Point, the zinc oxide feed addictive that particle diameter is 40-80 mesh is collected, metering, is put in storage at packaging after the assay was approved.
Embodiment 6
Prepare zinc oxide feed addictive
By 485kg hydrophobicity capsule material (201kg monoglyceride, 134kg hydrogenated oil and fat and 150kg palm oil), 100kg hydrophily capsule
Material (PEG1000) is put into collet heating tank respectively to be melted, and controlling jacket temperature processed is 125 DEG C, by the hydrophobicity capsule after fusing
Material and hydrophily capsule material are transferred in collet stirring homogeneous tank, and maintaining the jacket temperature of stirring homogeneous tank is 90 DEG C, starting stirring
Device, while 915kg crude zinc oxide materials (zinc oxide content 95wt%) are added, start Homogenizing pump after mixing evenly, keeps material mixed
Close uniformly, obtain mixture, then send the mixture to centrifugal spray tower, control the inlet air temperature of the centrifugal spray tower≤
5 DEG C, centrifugal turntable speed is 3800r/min, air quantity 40000m2/ min obtains zinc oxide feed addictive particle, finally makes
With concussion sieve screening, the zinc oxide feed addictive that particle diameter is 40-80 mesh is collected, metering, enters packaging after the assay was approved
Library.
Embodiment 7
Prepare zinc oxide feed addictive
By 364kg hydrophobicity capsule material (122kg monoglyceride, 82kg hydrogenated oil and fat and 160kg peanut oil), 76kg hydrophily capsule material
(PEG4000) it puts into collet heating tank and melts respectively, controlling jacket temperature processed is 130 DEG C, by the hydrophobicity capsule material after fusing
It is transferred in collet stirring homogeneous tank with hydrophily capsule material, maintaining the jacket temperature of stirring homogeneous tank is 90 DEG C, start blender,
1060kg crude zinc oxide materials (zinc oxide content 95wt%) are added simultaneously, starts Homogenizing pump after mixing evenly, mixes material
Uniformly, mixture is obtained, then the mixture is sent to centrifugal spray tower, controls inlet air temperature≤5 of the centrifugal spray tower
DEG C, centrifugal turntable speed is 4000r/min, air quantity 38000m2/ min obtains zinc oxide feed addictive particle, finally makes
With concussion sieve screening, the zinc oxide feed addictive that particle diameter is 40-80 mesh is collected, metering, enters packaging after the assay was approved
Library.
Embodiment 8
(in-vitro simulated gastric juice I is external for simulate the gastric juice in vitro for the zinc oxide feed addictive prepared in measurement embodiment 4
Simulate the gastric juice II) in disintegration and dissolution rate
(1) the zinc oxide feed addictive sample prepared in accurately weighed 2g embodiment 4 respectively is placed in two stripping rotors,
Using blade method, blade (since oxidation zinc weight proportion is big, and is easy to reunite, sample is prevented to be deposited on close to stripping rotor bottom as far as possible
Bottom of a cup portion), then the in-vitro simulated gastric juice of 400mL (in-vitro simulated gastric juice I or in-vitro simulated gastric juice are separately added into two stripping rotors
II), first stripping rotor takes a part of solution, is labeled as to stop operating after the rotational speed 1h of 100r/min at 37 DEG C
Mother liquor I is separately taken a part of solution to be centrifuged after 10min with the speed of 6000r/min and takes supernatant, marks supernatant I；Second molten
Cup takes a part of solution to stop operating after the rotational speed 2h of 100r/min at 37 DEG C out, is labeled as mother liquor II, separately takes one
Part solution is centrifuged after 10min with the speed of 6000r/min and takes supernatant, marks supernatant II；
(2) it takes 25.00mL mother liquor I and mother liquor II to be respectively placed in 50mL volumetric flask respectively, is separately added into 10mL dilute hydrochloric acid,
The zinc oxide feed addictive that is vortexed into mother liquor I and mother liquor II all dissolves, and shakes up, presses after being then diluted with water to scale respectively
HG/T 2792-2011 is titrated and is calculated, and test result is shown in Table 6.
(3) 25.00mL supernatant I and supernatant II is taken to be respectively placed in 250mL conical flask respectively, by HG/T 2792-
2011, it is titrated and is calculated, test result is shown in Table 7.
Using crude zinc oxide materials (zinc oxide content 95wt%) as control, successively according to step (1), step (3) and (4)
It is handled.
Embodiment 9
The zinc oxide feed addictive for preparing is disintegrated in simulated intestinal fluid and dissolution rate in vitro in measurement embodiment 4
(1) the zinc oxide feed addictive sample prepared in accurately weighed 2g embodiment 4 respectively is placed in five stripping rotors,
Using blade method, blade (since oxidation zinc weight proportion is big, and is easy to reunite, sample is prevented to be deposited on close to stripping rotor bottom as far as possible
Bottom of a cup portion), then add the in-vitro simulated intestinal juice of 400mL respectively into five stripping rotors, first stripping rotor is at 37 DEG C with 100r/
It stops operating after the rotational speed 1h of min, takes a part of solution, be labeled as mother liquor I, separately take a part of solution with 6000r/min
Speed centrifugation 10min after take supernatant, mark supernatant I；Second stripping rotor is turned at 37 DEG C with the revolving speed of 100r/min
It stops operating after dynamic 3h, takes a part of solution, be labeled as mother liquor II, a part of solution is separately taken to be centrifuged with the speed of 6000r/min
Supernatant is taken after 10min, marks supernatant II；Third stripping rotor is at 37 DEG C to stop after the rotational speed 5h of 100r/min
Rotation, takes a part of solution, is labeled as mother liquor III, takes after separately taking a part of solution to be centrifuged 10min with the speed of 6000r/min
Clear liquid marks supernatant III；4th stripping rotor, to stop operating after the rotational speed 7h of 100r/min, takes one at 37 DEG C
Divide solution, be labeled as mother liquor IV, separately takes a part of solution to be centrifuged after 10min with the speed of 6000r/min and take supernatant, on label
Clear liquid IV；5th stripping rotor, to stop operating after the rotational speed 9h of 100r/min, takes a part of solution at 37 DEG C, label
For mother liquor V, separately takes a part of solution to be centrifuged after 10min with the speed of 6000r/min and take supernatant, mark supernatant V；
(2) 25.00mL mother liquor I, mother liquor II, mother liquor III, mother liquor IV and mother liquor V is respectively taken to be respectively placed in 50mL volumetric flask,
It is separately added into 10mL dilute hydrochloric acid again, be vortexed the zinc oxide feed addition into mother liquor I, mother liquor II, mother liquor III, mother liquor IV and mother liquor V
Agent is all dissolved, and is shaken up after being then diluted with water to scale respectively, by HG/T 2792-2011, is titrated and calculated, and is tested
It the results are shown in Table 6.
(3) 25.00mL supernatant I, supernatant II, clear liquid III, supernatant IV and supernatant V is respectively taken to be respectively placed in 250mL
In conical flask, by HG/T 2792-2011, is titrated and calculated, test result is shown in Table 7.
Using crude zinc oxide materials (zinc oxide content 95wt%) as control, accurately weighed 2g crude zinc oxide materials are placed in dissolution
In cup, using blade method, blade (since oxidation zinc weight proportion is big, and is easy to reunite, prevents sample heavy close to stripping rotor bottom as far as possible
Product is in bottom of a cup portion), then into stripping rotor plus the in-vitro simulated intestinal juice of 400mL, at 37 DEG C with the rotational speed 1h of 100r/min after
It stops operating, takes a part of solution, be labeled as mother liquor, taken after separately taking a part of solution to be centrifuged 10min with the speed of 6000r/min
Supernatant marks supernatant；It takes 25.00mL mother liquor to be placed in 50mL volumetric flask, adds 10mL dilute hydrochloric acid, be vortexed into mother liquor
Crude zinc oxide materials all dissolve, and shake up after being then diluted with water to scale, by HG/T 2792-2011, are titrated and calculated,
Test result is shown in Table 6；It takes 25.00mL supernatant to be placed in 250mL conical flask, by HG/T 2792-2011, is titrated and counted
It calculates, test result is shown in Table 7.
Total zinc (Zn that the zinc oxide feed addictive prepared in 6 embodiment 4 of table dissolves out in simulation gastro-intestinal Fluid2+And ZnO)
Percentage
The Zn that the zinc oxide feed addictive prepared in 7 embodiment 4 of table dissolves out in simulation gastro-intestinal Fluid2+Percentage
The zinc oxide feed addictive prepared in 8 embodiment 4 of table, which is simulated in vitro in gastro-intestinal Fluid, to be disintegrated but is not converted into Zn2+
ZnO amount
Data in table 6 reflect the degree that zinc oxide feed addictive simulates disintegration release ZnO in gastro-intestinal Fluid in vitro,
With ZnO in solution and molecule Zn2+Total zinc dissolution percentage evaluation.Data in table 7 reflect zinc oxide feed addictive and exist
In in-vitro simulated gastro-intestinal Fluid after disintegration release ZnO, ZnO is partially converted into Zn2+Dissolution degree, with Zn in solution2+Dissolution hundred
Divide than evaluation.The total zinc percentage dissolved out in in-vitro simulated gastro-intestinal Fluid subtracts the Zn of dissolution2+Zinc oxide feeding can be obtained in percentage
Feed additives, which are simulated in vitro in gastro-intestinal Fluid, to be disintegrated but is not converted into Zn2+The amount of ZnO (amount and residue of ZnO are solid in dissolution fluid
The amount of ZnO in shape object), specific data are shown in Table 8.
By table 6 to table 8 it is found that zinc oxide feed addictive is in simulate the gastric juice I, though it is disintegrated the big portion absolutely the ZnO released
Divide and is converted to Zn2+, but still have in remaining solid content 69% ZnO, still there is 44% ZnO not to be disintegrated release after 2h, be not disintegrated with
The ZnO total amount not dissolved out is disintegrated still 50% or more；Only have 31% disintegration release in 1h in simulate the gastric juice II, but is converted to
Zn2+Only the 3.47% of dissolution, the amount about 68% of remaining solid content ZnO ZnO and disintegration but do not dissolve out in remaining solid content
ZnO amount is 96.5%, 2h still up to 89%；Significantly larger than crude zinc oxide materials cross after stomach the amount for entering the ZnO of enteron aisle.
Zinc oxide feed addictive has 60% disintegration release in simulated intestinal fluid in 9h, be converted into Zn2+Dissolution only has
8.7%, crude zinc oxide materials are all disintegrated after release in simulated intestinal fluid also only 4% is converted into Zn2+.Illustrate to be converted into ZnO
Zn2+Process occur mainly in gastric juice especially highly acid gastric juice.
Total ZnO surplus is only 9.67% to crude zinc oxide materials after 1h in simulate the gastric juice I, total after 1h in simulate the gastric juice II
ZnO surplus is also only 33.08%.And total ZnO surplus is zinc oxide feed addictive after 1h in simulate the gastric juice I
Total ZnO surplus is 50.37% after 69.23%, 2h；After total ZnO surplus is 96.53%, 2h after 1h in simulate the gastric juice II
Total ZnO surplus is 89.0%.Compared with crude zinc oxide materials, zinc oxide feed addictive is in simulate the gastric juice I and simulate the gastric juice II
Remaining ZnO total amount increases 59.56%, 63.45% respectively after middle 1h, it is sufficient to illustrate the oxygen prepared by molecular microcapsule technology
Change zinc feed additive and preferably protect ZnO in gastric juice, reduces the disintegration dissolution of ZnO under one's belt, keep the molecule of ZnO
State, particle crosses stomach, and only partial disintegration dissolution is converted into Zn2+, residual drug continues disintegration dissolution after entering enteron aisle, most of with ZnO
Molecular forms exist, and can preferably play enteron aisle anti-CaM antibody.
Embodiment 10
Influence of the zinc oxide feed addictive to diarrhea of weaned piglets in the verifying present invention
(1) test material
The zinc oxide feed addictive of the embodiment of the present invention 4: contain zinc oxide >=40%；
Feeding zinc oxide: Zn content >=76.3%, Hebei Bo Tai Environmental Protection Technology Co., Ltd；
Concentrated food stuff is produced by Henan silver hair animal husbandry Co., Ltd.
(2) experimental animal and processing design
Test selects 512, and parity is close, and kind is identical, and weight is suitable, the fifty-fifty three way cross weanling pig of male and female,
5 processing are randomly divided into, each processing group male and female is fifty-fifty, and specific processing design is shown in Table 9, experimental period 14d.
The tentative weanling pig of table 9 treats packet transaction design
(3) feeding management
Test pig uses stable breeding, during which feeds dry mash, is freely eaten and drinks water.Temperature controls the phase between 25-30 DEG C
To humidity 40-50%.It is daily to observe swinery health and mental status according to weanling pig routine immunization program and feeding management.
(4) observation and index test
1) behavior observation
The observation of the following contents: body temperature, the colour of skin, hair color, excrement shape and color is carried out daily；The state of mind；Incidence with
Improvement processing.
2) diarrhea is observed
During test, timing daily is observed and records grice diarrhoea head time and the course of disease in detail, calculates diarrhea rate.
Diarrhea rate=(head number × total of Diarrhoea days/test pig number × test number of days of experimental period diarrhea pig) ×
100%
3) other observations
The death rate: each processing group calculates the death rate.
(5) test results and analysis
512 weanling pigs are selected in test, and average just starting weight is 7.19kg/ head, and one-way analysis of variance is without significant difference
(p=0.927 > 0.05).The daily diarrhea rate of each group weanling pig is counted, monitors different dosing group to grice diarrhoea
It influences, test data is shown in Table 10, and the 7 days diarrhea rates in each test group weanling pig front and back are shown in Table 11 and Fig. 1, Fig. 2, and each test group is disconnected
Milk piglet whole process diarrhea rate, the death rate are shown in Table 12, and whole diarrhea rate histogram is shown in Fig. 3.
Each test group weanling pig day diarrhea rate statistics of table 10
| Processing group | No. 1 group (%) | No. 2 groups (%) | No. 3 groups (%) | No. 4 groups (%) | No. 5 groups (%) |
| 1st day | 2.88 | 2.88 | 1.92 | 2.00 | 7.00 |
| 2nd day | 4.81 | 7.69 | 6.73 | 7.00 | 13.00 |
| 3rd day | 9.62 | 3.85 | 10.58 | 10.00 | 14.00 |
| 4th day | 15.38 | 8.65 | 19.23 | 11.00 | 13.00 |
| 5th day | 9.62 | 8.65 | 16.35 | 10.00 | 10.00 |
| 6th day | 5.77 | 4.81 | 11.54 | 3.00 | 15.00 |
| 7th day | 2.88 | 5.77 | 5.77 | 4.00 | 13.00 |
| 8th day | 2.88 | 3.85 | 1.92 | 3.00 | 5.00 |
| 9th day | 1.92 | 4.81 | 0.96 | 4.00 | 4.00 |
| 10th day | 1.92 | 1.92 | 0.00 | 2.00 | 0.00 |
| 11st day | 0.96 | 0.00 | 0.96 | 1.00 | 0.00 |
| 12nd day | 0.00 | 0.96 | 0.96 | 0.00 | 2.00 |
| 13rd day | 0.96 | 1.92 | 0.96 | 0.00 | 1.00 |
| 14th day | 0.00 | 0.00 | 0.96 | 0.00 | 0.00 |
As shown in Table 10, No. 1, No. 2, No. 3, No. 4 groups diarrhea rate highest on day 4, wherein No. 1 group and No. 3 group diarrhea rates
Highest, respectively 15.38% and 19.23%, but since the 5th day, diarrhea rate is decreased obviously, and adds common feeding oxygen merely
7 days diarrhea rates maintain always higher level before changing No. 5 groups of zinc.From the 4th day to the 7th day, No. 1 group diarrhea rate is by under 15.38%
It is down to 2.88%, No. 3 group diarrhea rates drop to 5.77% by 19.23%, and No. 4 group diarrhea rates drop to 4% by 11%, significantly
The 7th day diarrhea rate 13% of lower than No. 5 groups illustrates that partial oxidation zinc feed additive is added in feed replaces common feeding oxygen
Obvious Antidiarrheic effect can be had in weaned piglet 7 days by changing zinc.
7 days diarrhea rate statistics before and after each test group weanling pig of table 11
| Processing | No. 1 group | No. 2 groups | No. 3 groups | No. 4 groups | No. 5 groups |
| Preceding 7 days diarrhea rate % | 7.55 | 6.04 | 10.44 | 7.14 | 12.43 |
| 7 days diarrhea rate % afterwards | 0.96 | 1.65 | 0.82 | 1.57 | 1.43 |
Chi-square analysis is carried out to 7 days diarrhea rates after weanling pig in table 11, as a result not significant (the p=0.719 of diarrhea rate difference
> 0.05), illustrate that a certain amount of zinc oxide feed addictive is added in feed certain prevention and treatment effect to diarrhea of weaned piglets
Fruit, from front and back, 7 days diarrhea of weaned piglets rates statistically can be seen that diarrhea of weaned piglets pressure is concentrated mainly on first 7 days, diarrhea rate
Height, and different dosing group diarrhea rate significant difference (p=0.001 < 0.05).But the 1 of zinc oxide feed addictive is added in test
Number, No. 3, before No. 4 groups 7 days diarrhea rates significantly lower than the common feeding zinc oxide of only addition convention amount No. 5 groups, though slightly higher addition is high
No. 2 groups of the feeding zinc oxide of dosage, but result difference is not significant (p=0.070 > 0.05).Wherein individually addition oxidation in test
No. 4 groups of 3000g/ tons of feeds of zinc feed additive, Zn content is only 900mg/kg, and preceding 7 days diarrhea rates are minimum, Antidiarrheic effect
It is best.
Each test group weanling pig whole process diarrhea rate of table 12, mortality statistics
Note: diarrhea does not occur for dead pig, dissects after dead no abnormal.
As shown in Table 12, each group adds different amount zinc oxide feed addictives and feeding zinc oxide is watched after feeding 14 days, addition
It each test group diarrhea rate of zinc oxide feed addictive and only adds feeding zinc oxide (No. 5 groups, 2900g/ tons) group and compares, diarrhea
Rate declines 2.67%, 1.30%, 2.57% respectively, declines obvious and significant difference (p=0.039 < 0.05), raises with only addition
It is compared with zinc oxide (No. 2 groups, 3900g/ tons) group, diarrhea rate illustrates to add in feed without significant difference (p=0.178 > 0.05)
Add certain amount zinc oxide feed addictive that can reduce diarrhea rate, reaches clinical effectiveness identical with the feeding zinc oxide of high dose.
A certain amount of zinc oxide feed addictive is added in feed can play certain Antidiarrheic effect to weanling pig.
Feed addition zinc oxide feed addictive 2250g per ton and feeding zinc oxide 1000g (containing Zn-ef ficiency 1435mg/kg), or oxidation
Zinc feed additive 1000g and feeding zinc oxide 1500g (containing Zn-ef ficiency 1440mg/kg) or zinc oxide feed addictive 3000g
(contain Zn-ef ficiency 900mg/kg) clinically can be substantially reduced diarrhea of weaned piglets rate, Antidiarrheic effect with containing Zn-ef ficiency about
The feeding zinc oxide effect of 3000mg/kg is suitable, wherein anti-to add 3000g/ tons of feeds of zinc oxide feed addictive in feed
Diarrhea effect is best.Zinc oxide feed addictive is individually or collocation uses the Zn-ef ficiency in feed while playing anti-CaM antibody
Content complies fully with No. 2625 bulletin requirement of The Ministry of Agriculture of the People's Republic of China, MOA.
Finally, it is stated that preferred embodiment above is only used to illustrate the technical scheme of the present invention and not to limit it, although logical
It crosses above preferred embodiment the present invention is described in detail, however, those skilled in the art should understand that, can be
Various changes are made to it in form and in details, without departing from claims of the present invention limited range.
Claims (9)
1. a kind of zinc oxide feed addictive, which is characterized in that by mass percentage, the additive includes following group grouping
At: hydrophobicity capsule material 24-58%, hydrophily capsule material 5-15%, zinc oxide 30-70%.
2. a kind of zinc oxide feed addictive as described in claim 1, which is characterized in that the hydrophobicity capsule material is single sweet
At least one of rouge, hydrogenated oil and fat, paraffin, palm oil or peanut oil.
3. a kind of zinc oxide feed addictive as described in claim 1, which is characterized in that the hydrophily capsule material is
At least one of PEG1000, PEG1500, PEG4000, PEG6000 or poloxamer.
4. a kind of preparation method of zinc oxide feed addictive described in any one of claims 1 to 3, which is characterized in that institute
State method specifically: mix after being respectively melted hydrophobicity capsule material and hydrophily capsule material, zinc oxide is then added, after mixing again
Mixture is obtained, the mixture is subjected to spray chilling.
5. method as claimed in claim 4, which is characterized in that the temperature of the fusing is 100-130 DEG C.
6. method as claimed in claim 4, which is characterized in that zinc oxide is added at 80-90 DEG C.
7. method as claimed in claim 4, which is characterized in that the spray chilling specifically: by the mixture send to from
Heart spray tower, controls inlet air temperature≤5 DEG C of the centrifugal spray tower, and centrifugal turntable speed is 3000-4000r/min, air quantity
For 30000-40000m3/min。
8. such as the described in any item methods of claim 4-7, which is characterized in that raise zinc oxide obtained after the spray chilling
Feed additives are sieved, and the zinc oxide feed addictive that particle diameter is 40-80 mesh is obtained.
9. a kind of zinc oxide feed addictive described in any one of claims 1 to 3 is preparing the application in feed.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111011611A (en) * | 2019-12-06 | 2020-04-17 | 金河生物科技股份有限公司 | Micro-capsule calcium chloride for dairy cows and preparation method and application thereof |
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