CN101431903A - Method for preparing ruminally protected choline - Google Patents

Method for preparing ruminally protected choline Download PDF

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Publication number
CN101431903A
CN101431903A CNA2006800544697A CN200680054469A CN101431903A CN 101431903 A CN101431903 A CN 101431903A CN A2006800544697 A CNA2006800544697 A CN A2006800544697A CN 200680054469 A CN200680054469 A CN 200680054469A CN 101431903 A CN101431903 A CN 101431903A
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choline
time
coatings
preparation according
ruminally protected
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CN101431903B (en
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李王植
金贤燮
李贤俊
奇光锡
朴修奉
金炫秀
奉相勋
洪全洙
郑暋噭
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Nuvo B & T Corp
Rural Development Administration Nat L
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Nuvo B & T Corp
Rural Development Administration Nat L
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    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23KFODDER
    • A23K40/00Shaping or working-up of animal feeding-stuffs
    • A23K40/30Shaping or working-up of animal feeding-stuffs by encapsulating; by coating
    • A23K40/35Making capsules specially adapted for ruminants
    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23KFODDER
    • A23K20/00Accessory food factors for animal feeding-stuffs
    • A23K20/10Organic substances
    • A23K20/158Fatty acids; Fats; Products containing oils or fats
    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23KFODDER
    • A23K20/00Accessory food factors for animal feeding-stuffs
    • A23K20/10Organic substances
    • A23K20/163Sugars; Polysaccharides
    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23KFODDER
    • A23K50/00Feeding-stuffs specially adapted for particular animals
    • A23K50/10Feeding-stuffs specially adapted for particular animals for ruminants
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61PSPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
    • A61P1/00Drugs for disorders of the alimentary tract or the digestive system
    • A61P1/16Drugs for disorders of the alimentary tract or the digestive system for liver or gallbladder disorders, e.g. hepatoprotective agents, cholagogues, litholytics
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61PSPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
    • A61P13/00Drugs for disorders of the urinary system
    • A61P13/12Drugs for disorders of the urinary system of the kidneys
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61PSPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
    • A61P21/00Drugs for disorders of the muscular or neuromuscular system
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61PSPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
    • A61P3/00Drugs for disorders of the metabolism
    • A61P3/02Nutrients, e.g. vitamins, minerals
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61PSPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
    • A61P43/00Drugs for specific purposes, not provided for in groups A61P1/00-A61P41/00

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  • General Chemical & Material Sciences (AREA)
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  • Nuclear Medicine, Radiotherapy & Molecular Imaging (AREA)
  • Animal Behavior & Ethology (AREA)
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  • Chemical Kinetics & Catalysis (AREA)
  • Bioinformatics & Cheminformatics (AREA)
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  • Urology & Nephrology (AREA)
  • Gastroenterology & Hepatology (AREA)
  • Fodder In General (AREA)
  • Feed For Specific Animals (AREA)
  • Acyclic And Carbocyclic Compounds In Medicinal Compositions (AREA)
  • Medicinal Preparation (AREA)

Abstract

The present invention relates to a method for preparing double-coated ruminally protected choline, which is not degraded by microorganisms, pH and water in the rumen, and thus can be stably delivered and absorbed in the lower digestive tract. More particularly, the method comprises the steps of: (a) preparing carrier-immobilized choline by immobilizing concentrated liquid choline on a carrier and then removing water from the immobilized choline; (b) preparing a first encapsulated choline by encapsulating the carrier-immobilized choline with a binder/coating material; (c) screening encapsulated choline having a size of 0.5-2.0mm from the first encapsulated choline; and (d) further encapsulating the screened encapsulated choline with any one or a combination of two or more selected from the group consisting of extremely hydrogenated oils and fats, and fatty acids having a melting point of more than 40 DEG C.

Description

The method for preparing ruminally protected choline
Technical field
The present invention relates to a kind of method for preparing ruminally protected choline, therefore described choline can be transported to lower digestive tract with being stabilized and also be absorbed therein not by the microorganism in the cud, pH and water degraded.Particularly, the present invention relates to a kind of method for preparing the ruminally protected choline of two coatings, comprise the following steps: that (a) is fixed on by the liquid choline that will concentrate from fixing choline, to remove moisture on the carrier then and prepare the fixing choline of carrier; (b) by choline with the fixing choline preparation encapsulation first time of bonding agent/coating material package carrier; (c) from the choline of encapsulation for the first time, screen encapsulated choline with 0.5-2.0mm size; (d) use and to be selected from down the encapsulated choline that organize any or two or more combination further encapsulate screening, its group comprises the oil or the fat of deep hydrogenation, and the aliphatic acid with the fusing point that is higher than 40 ℃.
Background technology
Known choline is a kind of necessary composition in some domestic animal researchs, but does not set up yet for the choline requirements of the cow that gives milk.And most of choline are degraded in the cud of ruminant, therefore have the needs of the technology that is not degraded for exploitation protection choline, make choline be absorbed and to use by cud and in small intestine.
To the lactation of choline response with to similar as response that must amino acid whose methionine, the classical symptom that choline lacks comprises that muscle weakens, the generation of fatty liver, kidney is hemorrhage and similar symptom.
Have found that by research choline is the limiting nutrient factor in the milk cow to the choline injection.And when choline lacked, owing to fatty liver appears in fat mechanism and the abnormal mechanism of secretion of liver, and when the injection of choline increased, the mobile increase of aliphatic acid caused reducing of fatty liver thus.
Reported that choline influences blood sugar, plasma cholesterol, serum insulin and serum N EFA (non-esterified fatty acid), greatly help to improve milk crop, the composition of milk, gain in weight and carcass proterties are degraded in cud but add the Choline Chloride major part in feed.
Ruminal microorganisms is degraded into choline and phosphoglycerol diester with the phosphatid ylcholine in the feed, and as intermediate metabolites choline is changed into methane and the choline of degrading via trimethylamine.As a result, only arrive small intestine in the known feed less than 1% choline.
Choline is the necessary nutrient in the livestock animals, but its effect can not be observed in ruminant, because it is degraded in cud.Owing to this reason, attempt to prevent that the trial that the choline composition is degraded from having carried out for a long time in cud.
For example, reported the encapsulated choline composition (US5,807,594) that is used for strengthening the increase of ruminant weight.But owing to be used as the various materials of the encapsulation reagent of choline composition, choline composition will be caused higher cost as the application of actual product.
Simultaneously, US 5,496, and 571 disclose the choline composition that can feed the encapsulation of the cow that gives milk, and US 5,190,775 discloses when feeding bioactivator such as choline through hydrophobic coating, can prevent that it is degraded in cud.But described patent does not advise preparing the ad hoc approach of composition, and does not provide enough protections that active material is not degraded by the ruminal microorganisms in the cud according to the simple coating with hydrophobic substance or the encapsulation of described patent yet.
And WO 94/15480 discloses with the encapsulated choline composition feeding of ruminant animals increases milk crop.But in this patent, hydrophobic coating also is used and does not mention specially the method that is used to prepare choline composition.In addition, WO 96/08168 discloses feed additive for ruminant, and it can be by being encapsulated in the liquid choline composition in the carrier and using aliphatic acid or the soap coating composition prepares.But its shortcoming is, when the liquid choline bag by during soap, soap can react with carbon dioxide in air.
In addition, it is known making choline keep stable lipid coatings (WO 03/059088A1) and two coating (US 2005/0019413A1) in cud.But the shortcoming of existence is the method complexity that forms coating.
As mentioned above, disclose and be used to strengthen that weight increases and the relevant many patents of choline composition of milk crop, and most of mention choline coated specific protection material, it is not degraded in cud.But these patents do not have openly to prepare specially the method for choline composition.
And, in the ruminally protected choline product that can buy from the market at present, there is the product that mixes and mixture is carried out the preparation of cooling spray step by with choline and protection material.But in this case, grown place cost height and installation cost height, and use and to have the perishing air of-60 ℃ of temperature, thereby cause the increase of production cost.
In addition, because product uses quick process for cooling to prepare, can form macropore (macro pores) in product, the operating condition that is used for production is also very complicated.In addition, the choline that is located on the ruminally protected choline product surface can not be protected, thereby causes the product effect to reduce.
Therefore, press for the technology of the choline composition of exploitation preparation coating, described stable against ruminal degradation also can be fed to ruminant.
Therefore, the present inventor has paid and made great efforts to solve the problem that choline is degraded greatly in ruminant tumor gastric.The result; the present inventor finds; ruminally protected choline by the preparation of following method is transported in the lower digestive tract with being stabilized and is absorbed therein and not by the microorganism in the cud, pH and water degraded; thereby finished the present invention: choline is fixed on the carrier and from fixing choline removes moisture; with this water-free choline of hydrophobic substance encapsulation; further encapsulate the choline of described encapsulation then with the material that is selected from down group: its group comprises the oil or the fat of deep hydrogenation, and the aliphatic acid with the fusing point that is higher than 40 ℃.
Summary of the invention
The object of the present invention is to provide a kind of method for preparing the ruminally protected choline of two coatings, described choline is not by the microorganism in the ruminant tumor gastric, pH and water degraded.
To achieve these goals, the invention provides a kind of method for preparing the ruminally protected choline of two coatings, this method comprises the following steps: that (a) is fixed on by the liquid choline that will concentrate and removes moisture on the carrier then prepare the fixing choline of carrier from fixing choline; (b) by choline with the fixing choline preparation encapsulation first time of bonding agent/coating material package carrier; (c) from the choline of encapsulation for the first time, screen encapsulated choline with 0.5-2.0mm size; (d) use and to be selected from down the encapsulated choline that organize any or two or more combination further encapsulate screening, its group comprises the oil or the fat of deep hydrogenation, and the aliphatic acid with the fusing point that is higher than 40 ℃.
By following detailed and appending claims, above-mentioned and other purposes of the present invention, feature and embodiment will be understood better.
The specific embodiment
The present invention relates to a kind of method for preparing the ruminally protected choline of two coatings, described choline by the microorganism in the ruminant tumor gastric, pH and water degraded, also is not absorbed thereby can be transported to lower digestive tract with being stabilized therein.
According to the present invention, in order to prepare two ruminally protected choline of coating, concentrated liquid choline is fixed on the carrier, then from wherein removing moisture with the fixing choline of preparation carrier.
From this angle, the liquid choline that concentrates is preferably and is selected from down a kind of in organizing or two or more mixture wherein, and its group comprises Choline Chloride, dihydrogen citrate choline, citric acid three choline and choline bitartrate.Carrier is preferably the water insoluble carrier that is selected from down group, comprises silicon, cellulose, starch and zeolite.More preferably carrier is a silicon.
Then, the fixing choline of carrier encapsulates to make the choline that graininess or needle-like encapsulate for the first time with binding agent/coating material.The packing of the choline that carrier is fixing is undertaken by extruder or screw extruder extruding mixture then by in blender such as ribbon mixer, general mixer, homogenizer or V-type blender fixing choline being mixed with binding agent/coating material and stirring.Here, choline and binding agent/coating material preferably are mixed with each other with the weight ratio of 1:0.1-2.0.And the porous plate in the extruder preferably has the size of 0.5-2.5mm, and the recipient in the extruder preferably to keep temperature be 10-60 ℃.
In addition, binding agent/coating material is preferably selected from down any of group or two or more mixture, and its group comprises unit price soap, divalence soap, and the aliphatic acid with the fusing point that is higher than 40 ℃.Unit price soap preferred fatty acid sodium or aliphatic acid potassium, divalence soap is preferably selected from down group, and its group comprises beeswax, PEG, surfactant, calcium stearate, zinc stearate and dolomol.Aliphatic acid with the fusing point that is higher than 40 ℃ is preferably selected from down group, comprises hydrogenated oil and fat, deep hydrogenation oil, palmitic acid and stearic acid.Hydrogenated oil and fat more preferably.
Then, from the choline of encapsulation for the first time, screen encapsulated choline with 0.5-2.0mm particle size.The encapsulated choline of screening further encapsulates with any or two or more the combination that is selected from down group, comprises deep hydrogenation oil and fat, and the aliphatic acid with the fusing point that is higher than 40 ℃, thus the preparation pair ruminally protected choline of coating.
The total amount of the two coating levels in the ruminally protected choline of two coatings of final preparation is compared photograph and is preferably 15-55% (w/w).
The advantage that the prepared in accordance with the present invention pair of ruminally protected choline of coating has is, it does not show the formation of macropore and has the shape of homogeneous, and macropore is the problem that exists in the product according to existing commercial cooling spray technology preparation.
And; the shortcoming that the product for preparing according to cooling spray technology has is; choline is positioned in microparticle surfaces; therefore reduced the stability in cud; and the advantage that the prepared in accordance with the present invention pair of ruminally protected choline of coating has is; because further carry out the coating second time (encapsulation) step through the choline product that contains that applies (encapsulation) step for the first time, the possibility that choline is distributed on the product surface reduces, so the most of choline that contain in the product can keep stable.In addition, the use of the cold-producing medium that the present invention need not use in cooling spray technology, thus reduced production cost, and require very low grown place and installation cost, make it reduce production cost of products.
When not having ruminally protected choline feeding of ruminant animals, great majority not have the choline of protection to be degraded in cud, make the effect of feeding choline be difficult to expection, cause choline to be wasted.On the other hand, when the ruminally protected choline of the stability with increase of being invented is used in aquaculture, it can increase the utilization of ruminant to nutrient, thereby can make the increase of livestock output, and shows the effect that increases in livestock.Therefore, ruminally protected choline of the present invention can help to produce the development of the feed addictive of functional livestock.
Embodiment
After this, with reference to embodiment the present invention further is described in detail.But, should be appreciated that these examples only are used to the purpose of explaining, and do not constitute restriction scope of the present invention.
Embodiment 1: the preparation of the choline that two coatings are ruminally protected
The liquid choline that concentrates is fixed on the carrier such as on silicon, cellulose, starch, zeolite or the analog, then moisture is wherein removed, and prepares the fixing choline of carrier thus.
Then, bonding agent/coating material such as beeswax, PEG, hydrogenated oil and fat or analog are joined in the fixing choline of carrier, then at blender such as fixing choline being mixed with binding agent/coating material in such as ribbon mixer, general mixer, homogenizer or V-type blender or similar device and stirring.Make mixture pass through extruder or screw extruder extruding, preparation encapsulates the choline of (coating) for the first time thus.Here, the temperature of the recipient in extruder or the screw extruder remains on 10-60 ℃.
In the choline of encapsulation for the first time, screening has the encapsulated choline of 0.5-2.0mm size.A kind of or two or more the combination that is selected from down group is joined in the choline of screening, its group comprises the oil or the fat of deep hydrogenation, aliphatic acid with the fusing point that is higher than 40 ℃, for example hydrogenation rape oil, hydrogenated corn oil, cotmar, hydrogenated groundnut, hydrogenation palm kernel oil, HPO, hydrogenated palm stearic acid, hydrogenation sunflower oil, hydrogenated rapeseed oil, palmitic acid and stearic acid.The mixture of the choline of encapsulation carries out the encapsulation step second time to containing for the first time in packaging system such as super mixer, ribbon mixer, roedige blender or fluid bed processor.Prepare two ruminally protected choline of coating thus.
Test case 1
With the liquid hydrogenated oil of 1kg (encapsulating material for the first time; Bonding agent/coating material) mixes with the 5kg choline, and the mixture of 1kg is pressed through porous plate with the preparation material of encapsulation for the first time with 1.0mm aperture.The encapsulating material first time of 1kg preparation is placed in the super mixer, then 670g is selected from liquid hydrogenated oil and has any in the aliphatic acid of the fusing point that is higher than 40 ℃ or two or more combination joins in the super mixer as encapsulating material for the second time, thus the material that preparation encapsulates for the second time.Here, for the second time the amount of encapsulating material be final production the encapsulation second time material gross weight 40.1%.
Test case 2
With the liquid hydrogenated oil of 1kg (encapsulating material for the first time; Bonding agent/coating material) mixes with the 5kg choline, and the mixture of 1kg is pressed through porous plate with the preparation material of encapsulation for the first time with 1.2mm aperture.The encapsulating material first time of 1kg preparation is placed in the super mixer, then 670g is selected from liquid hydrogenated oil and has any in the aliphatic acid of the fusing point that is higher than 40 ℃ or two or more combination joins in the super mixer as encapsulating material for the second time, thus the material that preparation encapsulates for the second time.Here, for the second time the amount of encapsulating material be final production the encapsulation second time material gross weight 40.1%.
Test case 3
With the liquid hydrogenated oil of 1kg (encapsulating material for the first time; Bonding agent/coating material) mixes with the 5kg choline, and the mixture of 1kg is pressed through porous plate with the preparation material of encapsulation for the first time with 1.5mm aperture.The encapsulating material first time of 1kg preparation is placed in the super mixer, then 670g is selected from liquid hydrogenated oil and has any in the aliphatic acid of the fusing point that is higher than 40 ℃ or two or more combination joins in the super mixer as encapsulating material for the second time, thus the material that preparation encapsulates for the second time.Here, for the second time the amount of encapsulating material be final production the encapsulation second time material gross weight 40.1%.
Test case 4
With the liquid hydrogenated oil of 1kg (encapsulating material for the first time; Bonding agent/coating material) mixes with the 5kg choline, and the mixture of 1kg is pressed through porous plate with the preparation material of encapsulation for the first time with 2.0mm aperture.The encapsulating material first time of 1kg preparation is placed in the super mixer, then 670g is selected from liquid hydrogenated oil and has any in the aliphatic acid of the fusing point that is higher than 40 ℃ or two or more combination joins in the super mixer as encapsulating material for the second time, thus the material that preparation encapsulates for the second time.Here, for the second time the amount of encapsulating material be final production the encapsulation second time material gross weight 40.1%.
Test case 5
With the unit price aliphatic acid of 1kg (encapsulating material for the first time; Bonding agent/coating material) mixes with the 5kg choline, and the mixture of 1kg is pressed through porous plate with the preparation material of encapsulation for the first time with 1.0mm aperture.The encapsulating material first time of 1kg preparation is placed in the super mixer, then 670g is selected from liquid hydrogenated oil and has any in the aliphatic acid of the fusing point that is higher than 40 ℃ or two or more combination joins in the super mixer as encapsulating material for the second time, thus the material that preparation encapsulates for the second time.Here, for the second time the amount of encapsulating material be final production the encapsulation second time material gross weight 40.1%.
Test case 6
With the PEG of 1kg (encapsulating material for the first time; Bonding agent/coating material) mixes with the 5kg choline, and the mixture of 1kg is pressed through porous plate with the preparation material of encapsulation for the first time with 1.0mm aperture.The encapsulating material first time of 1kg preparation is placed in the super mixer, then 670g is selected from liquid hydrogenated oil and has any in the aliphatic acid of the fusing point that is higher than 40 ℃ or two or more combination joins in the super mixer as encapsulating material for the second time, thus the material that preparation encapsulates for the second time.Here, for the second time the amount of encapsulating material be final production the encapsulation second time material gross weight 40.1%.
Test case 7
With the Tween 80 of 1kg (encapsulating material for the first time; Bonding agent/coating material) mixes with the 5kg choline, and the mixture of 1kg is pressed through porous plate with the preparation material of encapsulation for the first time with 1.0mm aperture.The encapsulating material first time of 1kg preparation is placed in the super mixer, then 670g is selected from liquid hydrogenated oil and has any in the aliphatic acid of the fusing point that is higher than 40 ℃ or two or more combination joins in the super mixer as encapsulating material for the second time, thus the material that preparation encapsulates for the second time.Here, for the second time the amount of encapsulating material be final production the encapsulation second time material gross weight 40.1%.
Test case 8
With the Span 80 of 1kg (encapsulating material for the first time; Bonding agent/coating material) mixes with the 5kg choline, and the mixture of 1kg is pressed through porous plate with the preparation material of encapsulation for the first time with 1.0mm aperture.The encapsulating material first time of 1kg preparation is placed in the super mixer, then 670g is selected from liquid hydrogenated oil and has any in the aliphatic acid of the fusing point that is higher than 40 ℃ or two or more combination joins in the super mixer as encapsulating material for the second time, thus the material that preparation encapsulates for the second time.Here, for the second time the amount of encapsulating material be final production the encapsulation second time material gross weight 40.1%.
Test case 9
With the liquid hydrogenated oil of 1kg (encapsulating material for the first time; Bonding agent/coating material) mixes with the 5kg choline, and the mixture of 1kg is pressed through porous plate with the preparation material of encapsulation for the first time with 1.2mm aperture.The encapsulating material first time of 1kg preparation is placed in the super mixer, then 500g is selected from liquid hydrogenated oil and has any in the aliphatic acid of the fusing point that is higher than 40 ℃ or two or more combination joins in the super mixer as encapsulating material for the second time, thus the material that preparation encapsulates for the second time.Here, for the second time the amount of encapsulating material be final production the encapsulation second time material gross weight 33.3%.
Test case 10
With the liquid hydrogenated oil of 1kg (encapsulating material for the first time; Bonding agent/coating material) mixes with the 5kg choline, and the mixture of 1kg is pressed through porous plate with the preparation material of encapsulation for the first time with 1.2mm aperture.The encapsulating material first time of 1kg preparation is placed in the super mixer, then 350g is selected from liquid hydrogenated oil and has any in the aliphatic acid of the fusing point that is higher than 40 ℃ or two or more combination joins in the super mixer as encapsulating material for the second time, thus the material that preparation encapsulates for the second time.Here, for the second time the amount of encapsulating material be final production the encapsulation second time material gross weight 25.9%.
Test case 11
With the liquid hydrogenated oil of 1kg (encapsulating material for the first time; Bonding agent/coating material) mixes with the 5kg choline, and the mixture of 1kg is pressed through porous plate with the preparation material of encapsulation for the first time with 1.2mm aperture.The encapsulating material first time of 1kg preparation is placed in the super mixer, then 250g is selected from liquid hydrogenated oil and has any in the aliphatic acid of the fusing point that is higher than 40 ℃ or two or more combination joins in the super mixer as encapsulating material for the second time, thus the material that preparation encapsulates for the second time.Here, for the second time the amount of encapsulating material be final production the encapsulation second time material gross weight 20.2%.
Test case 12
With the liquid hydrogenated oil of 1kg (encapsulating material for the first time; Bonding agent/coating material) mixes with the 5kg choline, and the mixture of 1kg is pressed through porous plate with the preparation material of encapsulation for the first time with 1.2mm aperture.The encapsulating material first time of 1kg preparation is placed in the super mixer, then 150g is selected from liquid hydrogenated oil and has any in the aliphatic acid of the fusing point that is higher than 40 ℃ or two or more combination joins in the super mixer as encapsulating material for the second time, thus the material that preparation encapsulates for the second time.Here, for the second time the amount of encapsulating material be final production the encapsulation second time material gross weight 13.0%.
Test case 13
With the liquid hydrogenated oil of 1kg (encapsulating material for the first time; Bonding agent/coating material) mixes with the 5kg choline, and the mixture of 1kg is pressed through porous plate with the preparation material of encapsulation for the first time with 1.2mm aperture.The encapsulating material first time of 1kg preparation is placed in the super mixer, then 50g is selected from liquid hydrogenated oil and has any in the aliphatic acid of the fusing point that is higher than 40 ℃ or two or more combination joins in the super mixer as encapsulating material for the second time, thus the material that preparation encapsulates for the second time.Here, for the second time the amount of encapsulating material be final production the encapsulation second time material gross weight 4.8%.
Test case 14
With the liquid hydrogenated oil of 2kg (encapsulating material for the first time; Bonding agent/coating material) mixes with the 4kg choline, and the mixture of 1kg is pressed through porous plate with the preparation material of encapsulation for the first time with 2.0mm aperture.The encapsulating material first time of 1kg preparation is placed in the super mixer, then 670g is selected from liquid hydrogenated oil and has any in the aliphatic acid of the fusing point that is higher than 40 ℃ or two or more combination joins in the super mixer as encapsulating material for the second time, thus the material that preparation encapsulates for the second time.Here, for the second time the amount of encapsulating material be final production the encapsulation second time material gross weight 40.1%.
Test case 15
With the liquid hydrogenated oil of 3kg (encapsulating material for the first time; Bonding agent/coating material) mixes with the 3kg choline, and the mixture of 1kg is pressed through porous plate with the preparation material of encapsulation for the first time with 2.0mm aperture.The encapsulating material first time of 1kg preparation is placed in the super mixer, then 670g is selected from liquid hydrogenated oil and has any in the aliphatic acid of the fusing point that is higher than 40 ℃ or two or more combination joins in the super mixer as encapsulating material for the second time, thus the material that preparation encapsulates for the second time.Here, for the second time the amount of encapsulating material be final production the encapsulation second time material gross weight 40.1%.
Embodiment 2: the external loss of ruminally protected choline
The external loss of every kind of two coating choline that prepare among the test case 1-15 is measured in the following manner, and measurement result shows in following table 1.
In order to be determined at the vitro stability of every kind of two coating choline that prepare among the test case 1-15, every kind of ruminally protected choline for preparing is placed in the test tube, distilled water is joined in the test tube, prepare 5% aqueous choline base solution.Use the many agitators of JEIO TECH MC-11 under 40 ℃ ± 0.1 ℃, this aqueous solution to be stirred 2 hours.
The aqueous solution that stirs is filtered so that only collect solid by No. 3 Whatman paper.Solid under 45 ℃ ± 0.1 ℃ dry at least 12 hours to remove remaining moisture fully.
With sample cool to room temperature in Sanpla Dry Keeper of drying, the sample that 300mg is cooled off is dissolved in chloroform and ethanol (1:1v/v) mixed solvent fully.Use 5%K 2CrO 4As indicator and solution 0.1N AgNO 3Measure the content of choline in the solution as titrant.
Shown measurement result in the following table 1.As shown in table 1, change very little or do not change (test case 1-4) according to the external choline loss of the variation of the hole dimension of porous plate.
About the kind of the encapsulating material first time, compare with the situation of using Tween 80 or Span80, using unit price aliphatic acid or divalence aliphatic acid PEG to show that the external loss of choline reduces under as the situation of the encapsulating material first time.As a result, can observe with using unit price aliphatic acid, divalence aliphatic acid PEG, Tween 80 or Span 80 and compare, liquid hydrogenated oil can cause the external loss of choline to reduce (test case 5-8) as encapsulating material for the first time.
About add the second time encapsulating material amount, added as can be seen the second time encapsulating material the increase of amount can make the external loss of choline reduce (test case 9-13).
And, about the first time encapsulating material with the ratio of choline, can observing for the first time, the ratio increase of encapsulating material and choline can make the external loss of choline reduce (test case 14 and 15).
Table 1
Test case External loss (%)
1 10.41
2 7.91
3 9.57
4 10.75
5 28.71
6 45.11
7 52.74
8 54.46
9 21.95
10 31.55
11 42.20
12 49.50
13 62.24
14 4.57
15 4.36
The result; can find; by selecting liquid hydrogenated oil as the encapsulating material first time; choline is mixed with the ratio of 1:0.5 or 1:1 with encapsulating material for the first time, mixture is carried out encapsulation step for the first time and use Ceng Jialiang the second time encapsulating material for the first time the material of encapsulation carry out the prepared ruminally protected choline demonstration of two coatings of encapsulation step for the second time and make external loss be reduced to minimum.
Embodiment 3: the nursing test of ruminally protected choline
Ruminally protected choline to preparation in the test case 15 carries out feeding in the body test, and this choline shows low external loss and has suitable size and high content of choline in the test of embodiment 2.
Feed test in order to use ruminally protected choline to carry out milk cow, select 10 cow heads that mediate lactation as test animal and give total mixing of mixed feed of q.s quantitative altogether, and serve as a large amount of nursings every day at interval 2 times with 12 hours.And ruminally protected choline (content of choline is 25%) is additionally fed cow with the amount (based on the 10g choline) of every cow 40g when the total mixing of nursing is quantitative.Twice of cow lactation every day and the mensuration output of milk.From the milk that is produced, obtain milk sample, and use the somatic number in automatic analyzer (LactoScopeR, MK2, DeltaInstruments, The Netherlands) mensuration milk constituents and the milk sample.
Measurement result shows in following table 2.As shown in table 2; therein ruminally protected choline is fed under the situation to cow; the day milk crop of cow is from feeding the 32.1kg after preceding 29.2kg is increased to nursing; increased by 9.9%; butter fat, milk proem, lactose and total solid have also increased by 7.9% respectively; 10.4%, 12.7% and 10.1%.And owing to fed ruminally protected choline, somatic number has descended 61.9% in the sample, drops to 103,000 cells/ml from 167,000 cells/ml, shows that ruminally protected choline is effective improving aspect the milk quality.In addition, in the sample total amount of content of choline comparison about 48.8% according to having increased, be increased to 66.75mg/ml from 44.85mg/ml, show that ruminally protected choline makes it can produce rich choline milk.
Table 2
Milk crop (kg/ days) Butter fat Milk proem Lactose Total solid Somatic number (10 3/ml) Choline (mg/ml)
Before the nursing 29.2 3.43% 2.79% 4.49% 11.57% 167 44.85
After the nursing 32.1 3.70% 3.08% 5.06% 12.74% 103 66.75
Content 109.9% 107.9% 110.4% 112.7% 110.1% 61.9% 148.8%
Industrial applicibility
As described in detail above, the invention provides a kind of method for preparing the ruminally protected choline of two coatings.Ruminally protected choline prepared in accordance with the present invention by the microorganism in the cud, pH and water degraded, also is not absorbed thereby can stably be transported in the lower digestive tract therein.And when it was used to raise ruminant domestic animal, it can increase the utilization of ruminant domestic animal to nutrient, thereby tame animal yield is increased, and made it can produce the function domestic animal of rich choline milk.In addition, the method that is used to prepare ruminally protected choline of the present invention can be used for protecting various compositions not ruminated degraded, and can be used for the production of various new feed additives.
Though the present invention is described in detail, it will be apparent to those skilled in the art that this description only is used for preferred implementation, rather than limit the scope of the invention with reference to special characteristic.Therefore, actual range of the present invention will be limited by the claims paid and equivalent thereof.

Claims (17)

1. method for preparing the ruminally protected choline of two coatings, this method comprises the following steps:
(a) be fixed on by the liquid choline that will concentrate and from fixing choline, remove moisture on the carrier then and prepare the fixing choline of carrier;
(b) by preparing encapsulated choline for the first time with the fixing choline of bonding agent/coating material package carrier;
(c) screen encapsulated choline from the first time the encapsulated choline with 0.5-2.0mm size; With
(d) use and to be selected from down the encapsulated choline that organize any or two or more combination further encapsulate screening, its group comprises the oil or the fat of deep hydrogenation, and the aliphatic acid with the fusing point that is higher than 40 ℃.
2, the method for the ruminally protected choline of the two coatings of preparation according to claim 1; it is characterized in that; the liquid choline that concentrates is to be selected from down a kind of in organizing or two or more mixture wherein, and its group comprises Choline Chloride, dihydrogen citrate choline, citric acid three choline and choline bitartrate.
3, the method for the ruminally protected choline of the two coatings of preparation according to claim 1 is characterized in that carrier is to be selected from down the water insoluble carrier of organizing, and its group comprises silicon, cellulose, starch and zeolite.
4, the method for the ruminally protected choline of the two coatings of preparation according to claim 1; it is characterized in that; binding agent/coating material is selected from down any of group or two or more mixture; its group comprises unit price soap; divalence soap, and aliphatic acid with the fusing point that is higher than 40 ℃.
5, the method for the ruminally protected choline of the two coatings of preparation according to claim 4 is characterized in that unit price soap is sodium soap or aliphatic acid potassium.
6, the method for the ruminally protected choline of the two coatings of preparation according to claim 4 is characterized in that, at least a during divalence soap is selected from down and organizes, and its group comprises beeswax, PEG, surfactant, calcium stearate, zinc stearate and dolomol.
7, the method for the ruminally protected choline of the two coatings of preparation according to claim 4 is characterized in that the aliphatic acid with the fusing point that is higher than 40 ℃ is selected from down group, and its group comprises hydrogenated oil and fat, deep hydrogenation oil, palmitic acid and stearic acid.
8, the method for the ruminally protected choline of the two coatings of preparation according to claim 1; it is characterized in that; the oil of described deep hydrogenation or fat and the aliphatic acid with the fusing point that is higher than 40 ℃ are selected from down group; its group comprises hydrogenation rape oil, hydrogenated corn oil, cotmar, hydrogenated groundnut, hydrogenation palm kernel oil, HPO, hydrogenated palm stearic acid, hydrogenation sunflower oil, hydrogenated rapeseed oil, palmitic acid and stearic acid.
9, the method for the ruminally protected choline of the two coatings of preparation according to claim 1 is characterized in that described choline and described binding agent/coating material are mixed with each other with the weight ratio of 1:0.1-2.0.
10, the method for the ruminally protected choline of the two coatings of preparation according to claim 1 is characterized in that step (b) comprising: mix in blender and stir fixing choline; In the extruding machine, encapsulate then.
11, the method for the ruminally protected choline of the two coatings of preparation according to claim 10 is characterized in that blender is selected from down group, and its group comprises ribbon mixer, general mixer, homogenizer and V-type blender.
12, the method for the ruminally protected choline of the two coatings of preparation according to claim 10 is characterized in that the extruding machine is extruder or screw extruder.
13, the method for the ruminally protected choline of the two coatings of preparation according to claim 1 is characterized in that the choline of encapsulation is graininess or needle-like for the first time.
14, according to the method for the ruminally protected choline of the two coatings of claim 10 or 12 described preparations, it is characterized in that the porous plate in the described extruding machine is of a size of 0.5-2.5mm.
15, the method for the ruminally protected choline of the two coatings of preparation according to claim 12 is characterized in that the temperature of the recipient in the described extruder remains on 10-60 ℃.
16, the method for the ruminally protected choline of the two coatings of preparation according to claim 1; it is characterized in that; step (d) is undertaken by the packaging system second time that is selected from down group, comprises super mixer, ribbon mixer, roedige blender and fluid bed processor.
17, the method for the ruminally protected choline of the two coatings of preparation according to claim 1 is characterized in that the total amount comparison of two coating levels is according to being 15-55% (w/w).
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