[go: up one dir, main page]

CN101431903B - Method for preparing ruminally protected choline - Google Patents

Method for preparing ruminally protected choline Download PDF

Info

Publication number
CN101431903B
CN101431903B CN2006800544697A CN200680054469A CN101431903B CN 101431903 B CN101431903 B CN 101431903B CN 2006800544697 A CN2006800544697 A CN 2006800544697A CN 200680054469 A CN200680054469 A CN 200680054469A CN 101431903 B CN101431903 B CN 101431903B
Authority
CN
China
Prior art keywords
choline
coatings
preparation according
protected
ruminally protected
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Expired - Fee Related
Application number
CN2006800544697A
Other languages
Chinese (zh)
Other versions
CN101431903A (en
Inventor
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
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Nuvo B&t Co ltd
RURAL DEV ADMINISTRATION NAT L
Original Assignee
Nuvo B&t Co ltd
RURAL DEV ADMINISTRATION NAT L
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Nuvo B&t Co ltd, RURAL DEV ADMINISTRATION NAT L filed Critical Nuvo B&t Co ltd
Publication of CN101431903A publication Critical patent/CN101431903A/en
Application granted granted Critical
Publication of CN101431903B publication Critical patent/CN101431903B/en
Expired - Fee Related legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Classifications

    • 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
    • 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
    • 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

Landscapes

  • Life Sciences & Earth Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Polymers & Plastics (AREA)
  • Engineering & Computer Science (AREA)
  • Food Science & Technology (AREA)
  • Zoology (AREA)
  • General Health & Medical Sciences (AREA)
  • Organic Chemistry (AREA)
  • Pharmacology & Pharmacy (AREA)
  • General Chemical & Material Sciences (AREA)
  • Animal Behavior & Ethology (AREA)
  • Medicinal Chemistry (AREA)
  • Public Health (AREA)
  • Veterinary Medicine (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Bioinformatics & Cheminformatics (AREA)
  • Nuclear Medicine, Radiotherapy & Molecular Imaging (AREA)
  • Animal Husbandry (AREA)
  • Birds (AREA)
  • Diabetes (AREA)
  • Obesity (AREA)
  • Hematology (AREA)
  • Nutrition Science (AREA)
  • Neurology (AREA)
  • Orthopedic Medicine & Surgery (AREA)
  • Physical Education & Sports Medicine (AREA)
  • Gastroenterology & Hepatology (AREA)
  • Urology & Nephrology (AREA)
  • Fodder In General (AREA)
  • Feed For Specific Animals (AREA)
  • Medicinal Preparation (AREA)
  • Acyclic And Carbocyclic Compounds In Medicinal Compositions (AREA)

Abstract

The present invention relates to a method for preparing ruminally protected choline, which is not degraded by microorganisms, pH and water in the rumen, and thus can be stably delivered to and absorbed in the lower digestive tract. In particular, the present invention relates to a method for preparing double-coated ruminally protected choline comprising the steps of: 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 or fats, and fatty acids having a melting point of higher than 40 ℃.

Description

制备反刍保护的胆碱的方法Process for preparing rumination-protected choline

技术领域 technical field

本发明涉及一种制备反刍保护的胆碱的方法,所述胆碱不被瘤胃中的微生物、pH和水降解,因此可被稳定地输送到下部消化道并在其中被吸收。具体地,本发明涉及一种制备双涂层反刍保护的胆碱的方法,包括下列步骤:(a)通过将浓缩的液体胆碱固定在载体上然后从固定的胆碱中除去水分来制备载体固定的胆碱;(b)通过用粘接剂/涂敷材料封装载体固定的胆碱制备第一次封装的胆碱;(c)从第一次封装的胆碱中筛选具有0.5-2.0mm尺寸的封装胆碱;和(d)使用选自下组的任何一种或者两种或多种的组合进一步封装筛选的封装胆碱,其组包括极度氢化的油或脂,以及具有高于40℃的熔点的脂肪酸。The present invention relates to a method for preparing rumination-protected choline, which is not degraded by microorganisms, pH and water in the rumen, and thus can be stably delivered to and absorbed in the lower digestive tract. Specifically, the present invention relates to a method for preparing double-coated ruminally protected choline comprising the steps of: (a) preparing the carrier by immobilizing concentrated liquid choline on the carrier and then removing water from the immobilized choline The choline of immobilization; (b) prepare the choline of encapsulation for the first time by the choline of immobilization of encapsulation carrier with adhesive/coating material; (c) screen the choline with 0.5-2.0mm from the choline of first encapsulation and (d) further encapsulate the screened encapsulated choline using any one or a combination of two or more selected from the group consisting of extremely hydrogenated oils or fats, and having a value higher than 40 Fatty acids with a melting point of °C.

背景技术 Background technique

已知胆碱是一些家畜研究中的一种必须成分,但对于产奶乳牛的胆碱需求仍未建立。而且,大多数胆碱在反刍动物的瘤胃中被降解,因此存在对于开发保护胆碱不被降解的技术的需要,使胆碱可通过瘤胃并在小肠中被吸收和使用。Choline is known to be an essential component in some livestock studies, but the choline requirement for lactating dairy cows remains unestablished. Also, most of choline is degraded in the rumen of ruminants, so there is a need to develop technology to protect choline from degradation so that choline can pass through the rumen and be absorbed and used in the small intestine.

对胆碱的哺乳响应与对作为必须氨基酸的蛋氨酸的响应类似,胆碱缺乏的典型症状包括肌肉减弱、脂肪肝的发生、肾脏出血以及类似症状。The lactational response to choline is similar to that to methionine, an essential amino acid, and typical symptoms of choline deficiency include muscle weakness, development of fatty liver, renal hemorrhage, and similar symptoms.

通过对胆碱注射的研究业已发现,胆碱是奶牛中的限制性营养因子。而且,在胆碱缺乏时,由于肝的脂肪机制和不正常的分泌机制而出现脂肪肝,并且当胆碱的注射增加时,脂肪酸的移动增加,由此导致脂肪肝的发生减少。Choline has been found to be the limiting nutritional factor in dairy cows through studies with choline injections. Also, in the case of choline deficiency, fatty liver occurs due to fatty mechanism and abnormal secretion mechanism of the liver, and when the injection of choline increases, the movement of fatty acid increases, thereby leading to a decrease in the occurrence of fatty liver.

已经报道胆碱影响血糖、血浆胆固醇、血清胰岛素和血清NEFA(非酯化脂肪酸),极大地有助于提高牛奶产量,牛奶的组成,增重量和屠体性状,但在饲料中添加氯化胆碱大部分在瘤胃中被降解。It has been reported that choline affects blood sugar, plasma cholesterol, serum insulin and serum NEFA (non-esterified fatty acids), which greatly contributes to the improvement of milk production, milk composition, weight gain and carcass traits, but the addition of choline chloride to the feed Bases are mostly degraded in the rumen.

反刍微生物将饲料中的磷脂酰胆碱降解成胆碱和磷酸甘油二酯,并且还经由三甲胺作为中间代谢物将胆碱转化成甲烷而降解胆碱。结果,已知饲料中只有不到1%的胆碱到达小肠。Ruminant microorganisms degrade phosphatidylcholine in feed to choline and phosphodiglycerides, and also degrade choline by converting choline to methane via trimethylamine as an intermediate metabolite. As a result, less than 1% of the choline in the diet is known to reach the small intestine.

胆碱是家畜动物中的必须养分,但其效果在反刍动物中不能被观察到,因为其在瘤胃中被降解。由于这种原因,试图防止胆碱成分在瘤胃中被降解的尝试已经进行了很长时间。Choline is an essential nutrient in livestock animals, but its effect cannot be observed in ruminants because it is degraded in the rumen. For this reason, attempts have been made for a long time to prevent the degradation of the choline component in the rumen.

例如,报道了用于加强反刍动物中重量增加的封装胆碱组合物(US5,807,594)。但是,由于被用作胆碱组合物的封装试剂的各种材料的原因,胆碱组合物作为实际产品的应用将招致较高的成本。For example, an encapsulated choline composition was reported for enhancing weight gain in ruminants (US 5,807,594). However, the application of the choline composition as an actual product will incur higher costs due to various materials used as an encapsulating agent for the choline composition.

同时,US5,496,571公开了可喂养产奶乳牛的封装的胆碱组合物,并且US5,190,775公开了当经过疏水涂层喂养生物活性物质诸如胆碱时,可防止其在瘤胃中被降解。但是,所述专利没有建议制备组合物的专门方法,并且根据所述专利的具有疏水物质的简单涂层或者封装也没有提供使活性物质不被瘤胃中的反刍微生物降解的足够保护。Meanwhile, US5,496,571 discloses encapsulated choline compositions that can be fed to lactating cows, and US5,190,775 discloses that biologically active substances such as choline can be prevented from being degraded in the rumen when fed through a hydrophobic coating. However, said patent does not suggest a specific method of preparing the composition, and a simple coating or encapsulation with a hydrophobic substance according to said patent does not provide sufficient protection of the active substance from degradation by ruminant microorganisms in the rumen.

而且,WO94/15480公开了用封装胆碱组合物喂养反刍动物来增加牛奶产量。但是,在该专利中,疏水涂层也被使用并且没有专门提及用于制备胆碱组合物的方法。此外,WO96/08168公开了反刍动物饲料添加剂,其可通过将液体胆碱组合物封装在载体中并使用脂肪酸或者脂肪酸盐包被组合物来制备。但是,其缺点是,当液体胆碱包被了脂肪酸盐时,脂肪酸盐可在空气中与二氧化碳发生反应。Furthermore, WO94/15480 discloses feeding ruminants an encapsulated choline composition to increase milk production. However, in this patent, a hydrophobic coating is also used and there is no specific mention of the method used to prepare the choline composition. Furthermore, WO96/08168 discloses a ruminant feed additive which can be prepared by encapsulating a liquid choline composition in a carrier and coating the composition with a fatty acid or fatty acid salt. However, its disadvantage is that when liquid choline is coated with fatty acid salt, fatty acid salt can react with carbon dioxide in the air.

另外,使胆碱在瘤胃中保持稳定的脂质涂层(WO03/059088A1)和双涂层(US2005/0019413A1)是已知的。但是,存在的缺点是形成涂层的方法复杂。In addition, a lipid coating (WO03/059088A1) and a double coating (US2005/0019413A1) to stabilize choline in the rumen are known. However, there is a disadvantage that the method of forming the coating is complicated.

如上所述,公开了与用于加强重量增加和牛奶产量的胆碱组合物有关的许多专利,并且大多数提到胆碱被涂敷了特定的保护物质,使其在瘤胃中不被降解。但是,这些专利没有专门公开制备胆碱组合物的方法。As mentioned above, many patents are published related to choline compositions for enhancing weight gain and milk production, and most mention that choline is coated with a specific protective substance so that it is not degraded in the rumen. However, these patents do not specifically disclose methods for preparing choline compositions.

而且,在目前可从市场上购买的反刍保护的胆碱产品中,存在通过将胆碱与保护物质混合并对混合物进行冷却喷雾步骤制备的产品。但是在这种情况下,生产地成本高以及安装成本高,并且使用具有-60℃温度的非常冷的空气,从而导致生产成本的增加。Also, among the rumination-protected choline products currently available on the market, there are products prepared by mixing choline with a protecting substance and subjecting the mixture to a cooling spraying step. In this case, however, production site costs are high and installation costs are high, and very cold air having a temperature of -60° C. is used, resulting in an increase in production costs.

此外,由于产品使用快速冷却工艺来制备,可在产品中形成大孔(macro pores),用于产品生产的操作条件也很复杂。另外,位于在反刍保护的胆碱产品表面上的胆碱不能得到保护,从而导致产品效果降低。In addition, since the product is prepared using a rapid cooling process, macro pores may be formed in the product, and operating conditions for product production are also complicated. In addition, the choline located on the surface of the rumination protected choline product cannot be protected, resulting in reduced product efficacy.

因此,迫切需要开发制备涂敷的胆碱组合物的技术,所述胆碱组合物对反刍降解稳定并可喂养给反刍动物。Therefore, there is an urgent need to develop techniques for preparing coated choline compositions that are stable against ruminant degradation and that can be fed to ruminants.

因此,本发明的发明人付出了极大的努力来解决胆碱在反刍动物瘤胃中降解的问题。结果,本发明的发明人发现,通过下述方法制备的反刍保护的胆碱被稳定地输送到下部消化道中并在其中被吸收而没有被瘤胃中的微生物、pH和水降解,从而完成了本发明:将胆碱固定在载体上并从固定的胆碱中除去水分,用疏水物质封装该不含水的胆碱,然后进一步用选自下组的物质封装所述封装的胆碱:其组包括极度氢化的油或脂,以及具有高于40℃的熔点的脂肪酸。Therefore, the inventors of the present invention have made great efforts to solve the problem of choline degradation in the rumen of ruminants. As a result, the inventors of the present invention found that rumination-protected choline prepared by the following method was stably delivered to and absorbed in the lower digestive tract without being degraded by microorganisms, pH, and water in the rumen, thereby completing the present invention. Invention: immobilizing choline on a carrier and removing water from the immobilized choline, encapsulating the non-aqueous choline with a hydrophobic substance, and then further encapsulating said encapsulated choline with a substance selected from the group consisting of Extremely hydrogenated oils or fats, and fatty acids with a melting point above 40°C.

发明内容 Contents of the invention

本发明的目的在于提供一种制备双涂层反刍保护的胆碱的方法,所述胆碱不被反刍动物瘤胃中的微生物、pH和水降解。The object of the present invention is to provide a process for the preparation of double-coated ruminally protected choline which is not degraded by microorganisms, pH and water in the rumen of ruminants.

为了实现上述目的,本发明提供了一种制备双涂层反刍保护的胆碱的方法,该方法包括下列步骤:(a)通过将浓缩的液体胆碱固定在载体上然后从固定的胆碱中除去水分制备载体固定的胆碱;(b)通过用粘接剂/涂敷材料封装载体固定的胆碱制备第一次封装的胆碱;(c)从第一次封装的胆碱中筛选具有0.5-2.0mm尺寸的封装胆碱;和(d)使用选自下组的任何一种或者两种或多种的组合进一步封装筛选的封装胆碱,其组包括极度氢化的油或脂,以及具有高于40℃的熔点的脂肪酸。In order to achieve the above object, the present invention provides a method for preparing double-coated ruminant-protected choline, the method comprising the following steps: (a) by immobilizing concentrated liquid choline on a carrier and then Remove moisture to prepare the choline immobilized by the carrier; (b) prepare the choline encapsulated for the first time by using the choline immobilized by the adhesive/coating material encapsulation carrier; (c) screen the choline with Encapsulated choline with a size of 0.5-2.0 mm; and (d) further encapsulating the screened encapsulated choline using any one or a combination of two or more selected from the group consisting of extremely hydrogenated oils or fats, and Fatty acids having a melting point above 40°C.

通过下面的详细描述和所附的权利要求书,本发明的上述和其他目的、特征和实施方式将会更好地被理解。The above and other objects, features and embodiments of the present invention will be better understood from the following detailed description and appended claims.

具体实施方式 Detailed ways

本发明涉及一种制备双涂层反刍保护的胆碱的方法,所述胆碱不被反刍动物瘤胃中的微生物、pH和水降解,从而可被稳定地输送到下部消化道并在其中被吸收。The present invention relates to a process for the preparation of double-coated ruminally protected choline, which is not degraded by microorganisms, pH and water in the rumen of ruminants, so that it can be stably delivered to and absorbed in the lower digestive tract .

根据本发明,为了制备双涂层反刍保护的胆碱,浓缩的液体胆碱被固定在载体上,然后从其中除去水分以制备载体固定的胆碱。According to the present invention, in order to prepare double-coated ruminant-protected choline, concentrated liquid choline is immobilized on a carrier, and then water is removed therefrom to prepare carrier-immobilized choline.

从这个角度讲,浓缩的液体胆碱优选为选自下组中的一种或者其中的两种或多种的混合物,其组包括氯化胆碱、柠檬酸二氢胆碱、柠檬酸三胆碱和酒石酸氢胆碱。载体优选为选自下组的水不溶性载体,包括硅、纤维素、淀粉和沸石。更优选载体为硅。From this point of view, the concentrated liquid choline is preferably selected from one of the following groups or a mixture of two or more thereof, which group includes choline chloride, dihydrocholine citrate, tricholine citrate base and choline bitartrate. The carrier is preferably a water-insoluble carrier selected from the group consisting of silicon, cellulose, starch and zeolite. More preferably the support is silicon.

然后,载体固定的胆碱用粘结剂/涂敷材料封装以制成颗粒状或针状第一次封装的胆碱。载体固定的胆碱的包装通过在混合器诸如螺条混合器、普通搅拌器、高速搅拌机或者V型混合器中将固定的胆碱与粘结剂/涂层材料混合并搅拌,然后通过挤压机或者螺旋挤压机挤压混合物来进行。这里,胆碱和粘结剂/涂敷材料优选以1:00.1-2.0的重量比彼此混合。而且,挤压机中的多孔板优选具有0.5-2.5mm的尺寸,并且挤压机中的挤压筒优选保持温度为10-60℃。Then, the carrier-immobilized choline is encapsulated with a binder/coating material to produce granular or needle-shaped first-encapsulated choline. The packaging of the carrier-immobilized choline is achieved by mixing and stirring the immobilized choline with the binder/coating material in a mixer such as a ribbon mixer, conventional blender, high-speed blender or V-blender, followed by extrusion extruder or screw extruder to extrude the mixture. Here, the choline and the binder/coating material are preferably mixed with each other in a weight ratio of 1:00.1-2.0. Also, the porous plate in the extruder preferably has a size of 0.5-2.5 mm, and the extruding cylinder in the extruder is preferably kept at a temperature of 10-60°C.

此外,粘结剂/涂敷材料优选选自下组的任何一种或者两种或多种的混合物,其组包括单价脂肪酸盐,二价脂肪酸盐,以及具有高于40℃的熔点的脂肪酸。单价脂肪酸盐优选脂肪酸钠或者脂肪酸钾,二价脂肪酸盐优选选自下组,其组包括蜂蜡、PEG、表面活性剂、硬脂酸钙、硬脂酸锌和硬脂酸镁。具有高于40℃的熔点的脂肪酸优选选自下组,包括氢化油、极度氢化油、软脂酸和硬脂酸。更优选的是氢化油。Furthermore, the binder/coating material is preferably any one or a mixture of two or more selected from the group consisting of monovalent fatty acid salts, divalent fatty acid salts, and fatty acid. The monovalent fatty acid salt is preferably fatty acid sodium or fatty acid potassium, and the divalent fatty acid salt is preferably selected from the group consisting of beeswax, PEG, surfactants, calcium stearate, zinc stearate and magnesium stearate. The fatty acid having a melting point above 40°C is preferably selected from the group consisting of hydrogenated oils, extremely hydrogenated oils, palmitic acid and stearic acid. More preferred are hydrogenated oils.

然后,从第一次封装的胆碱中筛选具有0.5-2.0mm粒子大小的封装胆碱。筛选的封装胆碱用选自下组的任何一种或者两种或多种的组合进一步封装,包括极度氢化油和脂,以及具有高于40℃的熔点的脂肪酸,由此制备双涂层反刍保护的胆碱。Then, the encapsulated choline having a particle size of 0.5-2.0 mm was screened from the first encapsulated choline. The screened encapsulated choline is further encapsulated with any one selected from the group or a combination of two or more, including extremely hydrogenated oils and fats, and fatty acids with a melting point higher than 40° C., thereby preparing a double-coated ruminant Protected choline.

最终制备的双涂层反刍保护的胆碱中的双涂层含量的总量比对照优选为15-55%(w/w)。The total amount of double coating content in the finally prepared double coating ruminant protected choline is preferably 15-55% (w/w) compared to the control.

根据本发明制备的双涂层反刍保护的胆碱具有的优点是,它不显示大孔的形成并具有均一的形状,而大孔是在根据现有商用冷却喷雾工艺制备的产品中存在的问题。The double-coated ruminant-protected choline prepared according to the present invention has the advantage that it does not exhibit the formation of macropores and has a uniform shape, which is a problem in products prepared according to existing commercial cooling spray processes .

而且,根据冷却喷雾工艺制备的产品具有的缺点是,胆碱被定位在微粒表面,因此降低了在瘤胃中的稳定性,而根据本发明制备的双涂层反刍保护的胆碱具有的优点在于,由于经过第一次涂敷(封装)步骤的含胆碱产品进一步进行第二次涂敷(封装)步骤,胆碱分布到产品表面上的可能性降低,因此产品中含有的大多数胆碱可保持稳定。另外,本发明并不需要在冷却喷雾工艺中使用的制冷剂的使用,从而降低了生产成本,并要求很低的生产地和安装成本,使其降低了产品的生产成本。Furthermore, products prepared according to the cooling spray process have the disadvantage that the choline is localized on the surface of the particles, thus reducing the stability in the rumen, whereas the double-coated rumen-protected choline prepared according to the present invention has the advantage that , since the choline-containing product after the first coating (encapsulation) step is further subjected to the second coating (encapsulation) step, the possibility of choline distribution on the surface of the product is reduced, so most of the choline contained in the product Can be kept stable. In addition, the present invention does not require the use of the refrigerant used in the cooling spray process, thereby reducing the production cost, and requires very low production site and installation costs, thereby reducing the production cost of the product.

当用没有反刍保护的胆碱喂养反刍动物时,大多数没有保护的胆碱将在瘤胃中被降解,使喂养胆碱的效果难以预期,导致胆碱浪费。另一方面,当所发明的具有增加的稳定性的反刍保护的胆碱在养殖业中被使用,其可增加反刍动物对养分的利用,从而可使牲畜产量的增加,并在牲畜中显示增加的功效。因此,本发明的反刍保护的胆碱可有助于能够生产功能性牲畜的饲料添加剂的发展。When feeding ruminants with choline without rumination protection, most of the choline without protection will be degraded in the rumen, making the effect of feeding choline unpredictable and resulting in choline waste. On the other hand, when the invented ruminant-protected choline with increased stability is used in the farming industry, it can increase the utilization of nutrients by ruminants, thereby enabling an increase in livestock production and showing increased effect. Therefore, the ruminant-protected choline of the present invention may contribute to the development of feed additives capable of producing functional livestock.

实施例Example

此后,将参照实施例对本发明进一步进行详细描述。但是,应当理解,这些例子仅仅用于解释的目的,而不构成对本发明的范围的限制。Hereinafter, the present invention will be described in further detail with reference to Examples. However, it should be understood that these examples are for illustrative purposes only and do not limit the scope of the invention.

实施例1:双涂层反刍保护的胆碱的制备Example 1: Preparation of choline for double-coated ruminant protection

浓缩的液体胆碱被固定在载体上诸如硅、纤维素、淀粉、沸石或者类似物上,然后将其中的水分除去,由此制备载体固定的胆碱。Concentrated liquid choline is immobilized on a carrier such as silicon, cellulose, starch, zeolite or the like, and then water is removed therefrom, thereby preparing carrier-immobilized choline.

然后,将粘接剂/涂敷材料诸如蜂蜡、PEG、氢化油或者类似物加入到载体固定的胆碱中,然后在混合器诸如诸如螺条混合器、普通搅拌器、高速搅拌机或者V型混合器或者类似装置中将固定的胆碱与粘结剂/涂层材料混合并搅拌。使混合物通过挤压机或者螺旋挤压机挤压,由此制备第一次封装(涂敷)的胆碱。这里,挤压机或者螺旋挤压机中的挤压筒的温度保持在10-60℃。Then, an adhesive/coating material such as beeswax, PEG, hydrogenated oil, or the like is added to the carrier-immobilized choline, and then mixed in a mixer such as a ribbon mixer, ordinary mixer, high-speed mixer, or V-type mixer. Mix and agitate the immobilized choline with the binder/coating material in a mixer or similar device. The mixture is extruded through an extruder or a screw extruder, thereby preparing first encapsulated (coated) choline. Here, the temperature of the extrusion barrel in the extruder or screw extruder is maintained at 10-60°C.

在第一次封装的胆碱中,筛选具有0.5-2.0mm尺寸的封装胆碱。将选自下组的一种或者两种或多种的组合加入到筛选的胆碱中,其组包括极度氢化的油或脂,具有高于40℃的熔点的脂肪酸,例如氢化菜油、氢化玉米油、氢化棉籽油、氢化花生油、氢化棕仁油、氢化棕榈油、氢化棕榈硬脂酸、氢化向日葵油、氢化菜籽油,软脂酸和硬脂酸。在封装装置诸如高速混合器、螺条混合器、roedige混合器或者流化床处理器中对含有第一次封装的胆碱的混合物进行第二次封装步骤。由此制备双涂层反刍保护的胆碱。Among the first encapsulated cholines, encapsulated cholines having a size of 0.5-2.0 mm were screened. Add one or a combination of two or more selected from the group consisting of extremely hydrogenated oils or fats, fatty acids with a melting point higher than 40°C, such as hydrogenated rapeseed oil, hydrogenated corn Oil, hydrogenated cottonseed oil, hydrogenated peanut oil, hydrogenated palm kernel oil, hydrogenated palm oil, hydrogenated palm stearic acid, hydrogenated sunflower oil, hydrogenated rapeseed oil, palmitic and stearic acids. The mixture containing the first encapsulated choline is subjected to a second encapsulation step in an encapsulation apparatus such as a high speed mixer, ribbon mixer, roedige mixer or fluid bed processor. A double-coated rumination-protected choline was thus prepared.

测试例1test case 1

将1kg的液体氢化油(第一次封装材料;粘接剂/涂敷材料)与5kg胆碱混合,并将1kg的混合物挤压通过具有1.0mm孔径的多孔板以制备第一次封装的材料。将1kg制备的第一次封装材料放置到高速混合器中,然后将670g选自液体氢化油和具有高于40℃的熔点的脂肪酸中的任何一种或者两种或多种的组合加入到高速混合器中作为第二次封装材料,从而制备第二次封装的材料。这里,第二次封装材料的量是最终生产的第二次封装的材料的总重量的40.1%。1 kg of liquid hydrogenated oil (primary encapsulation material; adhesive/coating material) was mixed with 5 kg of choline, and 1 kg of the mixture was extruded through a perforated plate with a pore diameter of 1.0 mm to prepare a primary encapsulation material . 1 kg of the first packaging material prepared is placed in a high-speed mixer, and then 670 g of any one or a combination of two or more selected from liquid hydrogenated oils and fatty acids with a melting point higher than 40° C. is added to the high-speed mixer. Mixer as the second encapsulation material, thereby preparing the second encapsulation material. Here, the amount of the second packaging material is 40.1% of the total weight of the final produced second packaging material.

测试例2test case 2

将1kg的液体氢化油(第一次封装材料;粘接剂/涂敷材料)与5kg胆碱混合,并将1kg的混合物挤压通过具有1.2mm孔径的多孔板以制备第一次封装的材料。将1kg制备的第一次封装材料放置到高速混合器中,然后将670g选自液体氢化油和具有高于40℃的熔点的脂肪酸中的任何一种或者两种或多种的组合加入到高速混合器中作为第二次封装材料,从而制备第二次封装的材料。这里,第二次封装材料的量是最终生产的第二次封装的材料的总重量的40.1%。1 kg of liquid hydrogenated oil (primary encapsulation material; adhesive/coating material) was mixed with 5 kg of choline, and 1 kg of the mixture was extruded through a perforated plate with a pore diameter of 1.2 mm to prepare a primary encapsulation material . 1 kg of the first packaging material prepared is placed in a high-speed mixer, and then 670 g of any one or a combination of two or more selected from liquid hydrogenated oils and fatty acids with a melting point higher than 40° C. is added to the high-speed mixer. Mixer as the second encapsulation material, thereby preparing the second encapsulation material. Here, the amount of the second packaging material is 40.1% of the total weight of the final produced second packaging material.

测试例3Test case 3

将1kg的液体氢化油(第一次封装材料;粘接剂/涂敷材料)与5kg胆碱混合,并将1kg的混合物挤压通过具有1.5mm孔径的多孔板以制备第一次封装的材料。将1kg制备的第一次封装材料放置到高速混合器中,然后将670g选自液体氢化油和具有高于40℃的熔点的脂肪酸中的任何一种或者两种或多种的组合加入到高速混合器中作为第二次封装材料,从而制备第二次封装的材料。这里,第二次封装材料的量是最终生产的第二次封装的材料的总重量的40.1%。1 kg of liquid hydrogenated oil (primary encapsulation material; adhesive/coating material) was mixed with 5 kg of choline, and 1 kg of the mixture was extruded through a perforated plate with a pore size of 1.5 mm to prepare a primary encapsulation material . 1 kg of the first packaging material prepared is placed in a high-speed mixer, and then 670 g of any one or a combination of two or more selected from liquid hydrogenated oils and fatty acids with a melting point higher than 40° C. is added to the high-speed mixer. Mixer as the second encapsulation material, thereby preparing the second encapsulation material. Here, the amount of the second packaging material is 40.1% of the total weight of the final produced second packaging material.

测试例4Test case 4

将1kg的液体氢化油(第一次封装材料;粘接剂/涂敷材料)与5kg胆碱混合,并将1kg的混合物挤压通过具有2.0mm孔径的多孔板以制备第一次封装的材料。将1kg制备的第一次封装材料放置到高速混合器中,然后将670g选自液体氢化油和具有高于40℃的熔点的脂肪酸中的任何一种或者两种或多种的组合加入到高速混合器中作为第二次封装材料,从而制备第二次封装的材料。这里,第二次封装材料的量是最终生产的第二次封装的材料的总重量的40.1%。1 kg of liquid hydrogenated oil (primary encapsulation material; adhesive/coating material) was mixed with 5 kg of choline, and 1 kg of the mixture was extruded through a perforated plate with a pore diameter of 2.0 mm to prepare a primary encapsulation material . 1 kg of the first packaging material prepared is placed in a high-speed mixer, and then 670 g of any one or a combination of two or more selected from liquid hydrogenated oils and fatty acids with a melting point higher than 40° C. is added to the high-speed mixer. Mixer as the second encapsulation material, thereby preparing the second encapsulation material. Here, the amount of the second packaging material is 40.1% of the total weight of the final produced second packaging material.

测试例5Test case 5

将1kg的单价脂肪酸(第一次封装材料;粘接剂/涂敷材料)与5kg胆碱混合,并将1kg的混合物挤压通过具有1.0mm孔径的多孔板以制备第一次封装的材料。将1kg制备的第一次封装材料放置到高速混合器中,然后将670g选自液体氢化油和具有高于40℃的熔点的脂肪酸中的任何一种或者两种或多种的组合加入到高速混合器中作为第二次封装材料,从而制备第二次封装的材料。这里,第二次封装材料的量是最终生产的第二次封装的材料的总重量的40.1%。1 kg of monovalent fatty acid (primary encapsulation material; adhesive/coating material) was mixed with 5 kg of choline, and 1 kg of the mixture was extruded through a perforated plate with a pore size of 1.0 mm to prepare a primary encapsulation material. 1 kg of the first packaging material prepared is placed in a high-speed mixer, and then 670 g of any one or a combination of two or more selected from liquid hydrogenated oils and fatty acids with a melting point higher than 40° C. is added to the high-speed mixer. Mixer as the second encapsulation material, thereby preparing the second encapsulation material. Here, the amount of the second packaging material is 40.1% of the total weight of the final produced second packaging material.

测试例6Test case 6

将1kg的PEG(第一次封装材料;粘接剂/涂敷材料)与5kg胆碱混合,并将1kg的混合物挤压通过具有1.0mm孔径的多孔板以制备第一次封装的材料。将1kg制备的第一次封装材料放置到高速混合器中,然后将670g选自液体氢化油和具有高于40℃的熔点的脂肪酸中的任何一种或者两种或多种的组合加入到高速混合器中作为第二次封装材料,从而制备第二次封装的材料。这里,第二次封装材料的量是最终生产的第二次封装的材料的总重量的40.1%。1 kg of PEG (primary encapsulating material; adhesive/coating material) was mixed with 5 kg of choline, and 1 kg of the mixture was extruded through a perforated plate having a pore diameter of 1.0 mm to prepare a primary encapsulating material. 1 kg of the first packaging material prepared is placed in a high-speed mixer, and then 670 g of any one or a combination of two or more selected from liquid hydrogenated oils and fatty acids with a melting point higher than 40° C. is added to the high-speed mixer. Mixer as the second encapsulation material, thereby preparing the second encapsulation material. Here, the amount of the second packaging material is 40.1% of the total weight of the final produced second packaging material.

测试例7Test case 7

将1kg的吐温80(第一次封装材料;粘接剂/涂敷材料)与5kg胆碱混合,并将1kg的混合物挤压通过具有1.0mm孔径的多孔板以制备第一次封装的材料。将1kg制备的第一次封装材料放置到高速混合器中,然后将670g选自液体氢化油和具有高于40℃的熔点的脂肪酸中的任何一种或者两种或多种的组合加入到高速混合器中作为第二次封装材料,从而制备第二次封装的材料。这里,第二次封装材料的量是最终生产的第二次封装的材料的总重量的40.1%。1 kg of Tween 80 (primary encapsulation material; adhesive/coating material) was mixed with 5 kg of choline, and 1 kg of the mixture was extruded through a perforated plate with a pore size of 1.0 mm to prepare a primary encapsulation material . 1 kg of the first packaging material prepared is placed in a high-speed mixer, and then 670 g of any one or a combination of two or more selected from liquid hydrogenated oils and fatty acids with a melting point higher than 40° C. is added to the high-speed mixer. Mixer as the second encapsulation material, thereby preparing the second encapsulation material. Here, the amount of the second packaging material is 40.1% of the total weight of the final produced second packaging material.

测试例8Test case 8

将1kg的Span80(第一次封装材料;粘接剂/涂敷材料)与5kg胆碱混合,并将1kg的混合物挤压通过具有1.0mm孔径的多孔板以制备第一次封装的材料。将1kg制备的第一次封装材料放置到高速混合器中,然后将670g选自液体氢化油和具有高于40℃的熔点的脂肪酸中的任何一种或者两种或多种的组合加入到高速混合器中作为第二次封装材料,从而制备第二次封装的材料。这里,第二次封装材料的量是最终生产的第二次封装的材料的总重量的40.1%。1 kg of Span80 (primary packaging material; adhesive/coating material) was mixed with 5 kg of choline, and 1 kg of the mixture was extruded through a perforated plate having a pore size of 1.0 mm to prepare a primary packaging material. 1 kg of the first packaging material prepared is placed in a high-speed mixer, and then 670 g of any one or a combination of two or more selected from liquid hydrogenated oils and fatty acids with a melting point higher than 40° C. is added to the high-speed mixer. Mixer as the second encapsulation material, thereby preparing the second encapsulation material. Here, the amount of the second packaging material is 40.1% of the total weight of the final produced second packaging material.

测试例9Test case 9

将1kg的液体氢化油(第一次封装材料;粘接剂/涂敷材料)与5kg胆碱混合,并将1kg的混合物挤压通过具有1.2mm孔径的多孔板以制备第一次封装的材料。将1kg制备的第一次封装材料放置到高速混合器中,然后将500g选自液体氢化油和具有高于40℃的熔点的脂肪酸中的任何一种或者两种或多种的组合加入到高速混合器中作为第二次封装材料,从而制备第二次封装的材料。这里,第二次封装材料的量是最终生产的第二次封装的材料的总重量的33.3%。1 kg of liquid hydrogenated oil (primary encapsulation material; adhesive/coating material) was mixed with 5 kg of choline, and 1 kg of the mixture was extruded through a perforated plate with a pore diameter of 1.2 mm to prepare a primary encapsulation material . 1 kg of the first packaging material prepared is placed in a high-speed mixer, and then 500 g of any one or a combination of two or more selected from liquid hydrogenated oils and fatty acids with a melting point higher than 40° C. is added to the high-speed mixer. Mixer as the second encapsulation material, thereby preparing the second encapsulation material. Here, the amount of the second packaging material is 33.3% of the total weight of the final produced second packaging material.

测试例10Test case 10

将1kg的液体氢化油(第一次封装材料;粘接剂/涂敷材料)与5kg胆碱混合,并将1kg的混合物挤压通过具有1.2mm孔径的多孔板以制备第一次封装的材料。将1kg制备的第一次封装材料放置到高速混合器中,然后将350g选自液体氢化油和具有高于40℃的熔点的脂肪酸中的任何一种或者两种或多种的组合加入到高速混合器中作为第二次封装材料,从而制备第二次封装的材料。这里,第二次封装材料的量是最终生产的第二次封装的材料的总重量的25.9%。1 kg of liquid hydrogenated oil (primary encapsulation material; adhesive/coating material) was mixed with 5 kg of choline, and 1 kg of the mixture was extruded through a perforated plate with a pore diameter of 1.2 mm to prepare a primary encapsulation material . 1 kg of the first packaging material prepared is placed in a high-speed mixer, and then 350 g of any one or a combination of two or more selected from liquid hydrogenated oils and fatty acids with a melting point higher than 40° C. is added to the high-speed mixer. Mixer as the second encapsulation material, thereby preparing the second encapsulation material. Here, the amount of the second packaging material is 25.9% of the total weight of the final produced second packaging material.

测试例11Test case 11

将1kg的液体氢化油(第一次封装材料;粘接剂/涂敷材料)与5kg胆碱混合,并将1kg的混合物挤压通过具有1.2mm孔径的多孔板以制备第一次封装的材料。将1kg制备的第一次封装材料放置到高速混合器中,然后将250g选自液体氢化油和具有高于40℃的熔点的脂肪酸中的任何一种或者两种或多种的组合加入到高速混合器中作为第二次封装材料,从而制备第二次封装的材料。这里,第二次封装材料的量是最终生产的第二次封装的材料的总重量的20.2%。1 kg of liquid hydrogenated oil (primary encapsulation material; adhesive/coating material) was mixed with 5 kg of choline, and 1 kg of the mixture was extruded through a perforated plate with a pore diameter of 1.2 mm to prepare a primary encapsulation material . 1 kg of the first packaging material prepared is placed in a high-speed mixer, and then 250 g of any one or a combination of two or more selected from liquid hydrogenated oils and fatty acids with a melting point higher than 40° C. is added to the high-speed mixer. Mixer as the second encapsulation material, thereby preparing the second encapsulation material. Here, the amount of the second packaging material is 20.2% of the total weight of the final produced second packaging material.

测试例12Test case 12

将1kg的液体氢化油(第一次封装材料;粘接剂/涂敷材料)与5kg胆碱混合,并将1kg的混合物挤压通过具有1.2mm孔径的多孔板以制备第一次封装的材料。将1kg制备的第一次封装材料放置到高速混合器中,然后将150g选自液体氢化油和具有高于40℃的熔点的脂肪酸中的任何一种或者两种或多种的组合加入到高速混合器中作为第二次封装材料,从而制备第二次封装的材料。这里,第二次封装材料的量是最终生产的第二次封装的材料的总重量的13.0%。1 kg of liquid hydrogenated oil (primary encapsulation material; adhesive/coating material) was mixed with 5 kg of choline, and 1 kg of the mixture was extruded through a perforated plate with a pore diameter of 1.2 mm to prepare a primary encapsulation material . 1 kg of the first packaging material prepared is placed in a high-speed mixer, and then 150 g of any one or a combination of two or more selected from liquid hydrogenated oils and fatty acids with a melting point higher than 40° C. is added to the high-speed mixer. Mixer as the second encapsulation material, thereby preparing the second encapsulation material. Here, the amount of the second packaging material is 13.0% of the total weight of the final produced second packaging material.

测试例13Test case 13

将1kg的液体氢化油(第一次封装材料;粘接剂/涂敷材料)与5kg胆碱混合,并将1kg的混合物挤压通过具有1.2mm孔径的多孔板以制备第一次封装的材料。将1kg制备的第一次封装材料放置到高速混合器中,然后将50g选自液体氢化油和具有高于40℃的熔点的脂肪酸中的任何一种或者两种或多种的组合加入到高速混合器中作为第二次封装材料,从而制备第二次封装的材料。这里,第二次封装材料的量是最终生产的第二次封装的材料的总重量的4.8%。1 kg of liquid hydrogenated oil (primary encapsulation material; adhesive/coating material) was mixed with 5 kg of choline, and 1 kg of the mixture was extruded through a perforated plate with a pore diameter of 1.2 mm to prepare a primary encapsulation material . 1 kg of the first packaging material prepared is placed in a high-speed mixer, and then 50 g of any one or a combination of two or more selected from liquid hydrogenated oils and fatty acids with a melting point higher than 40° C. is added to the high-speed mixer. Mixer as the second encapsulation material, thereby preparing the second encapsulation material. Here, the amount of the second packaging material is 4.8% of the total weight of the final produced second packaging material.

测试例14Test case 14

将2kg的液体氢化油(第一次封装材料;粘接剂/涂敷材料)与4kg胆碱混合,并将1kg的混合物挤压通过具有2.0mm孔径的多孔板以制备第一次封装的材料。将1kg制备的第一次封装材料放置到高速混合器中,然后将670g选自液体氢化油和具有高于40℃的熔点的脂肪酸中的任何一种或者两种或多种的组合加入到高速混合器中作为第二次封装材料,从而制备第二次封装的材料。这里,第二次封装材料的量是最终生产的第二次封装的材料的总重量的40.1%。2 kg of liquid hydrogenated oil (primary encapsulation material; adhesive/coating material) was mixed with 4 kg of choline, and 1 kg of the mixture was extruded through a perforated plate with a pore size of 2.0 mm to prepare a primary encapsulation material . 1 kg of the first packaging material prepared is placed in a high-speed mixer, and then 670 g of any one or a combination of two or more selected from liquid hydrogenated oils and fatty acids with a melting point higher than 40° C. is added to the high-speed mixer. Mixer as the second encapsulation material, thereby preparing the second encapsulation material. Here, the amount of the second packaging material is 40.1% of the total weight of the final produced second packaging material.

测试例15Test case 15

将3kg的液体氢化油(第一次封装材料;粘接剂/涂敷材料)与3kg胆碱混合,并将1kg的混合物挤压通过具有2.0mm孔径的多孔板以制备第一次封装的材料。将1kg制备的第一次封装材料放置到高速混合器中,然后将670g选自液体氢化油和具有高于40℃的熔点的脂肪酸中的任何一种或者两种或多种的组合加入到高速混合器中作为第二次封装材料,从而制备第二次封装的材料。这里,第二次封装材料的量是最终生产的第二次封装的材料的总重量的40.1%。3 kg of liquid hydrogenated oil (primary encapsulation material; adhesive/coating material) was mixed with 3 kg of choline, and 1 kg of the mixture was extruded through a perforated plate with a pore size of 2.0 mm to prepare a primary encapsulation material . 1 kg of the first packaging material prepared is placed in a high-speed mixer, and then 670 g of any one or a combination of two or more selected from liquid hydrogenated oils and fatty acids with a melting point higher than 40° C. is added to the high-speed mixer. Mixer as the second encapsulation material, thereby preparing the second encapsulation material. Here, the amount of the second packaging material is 40.1% of the total weight of the final produced second packaging material.

实施例2:反刍保护的胆碱的体外损失Example 2: In vitro loss of choline for rumination protection

测试例1-15中制备的每种双涂层胆碱的体外损失以下列方式测定,测定结果在下表1中显示。The in vitro loss of choline of each double-coated layer prepared in Test Examples 1-15 was measured in the following manner, and the results of the measurement are shown in Table 1 below.

为了测定在测试例1-15中制备的每种双涂层胆碱的体外稳定性,将每种制备的反刍保护的胆碱放置在试管中,将蒸馏水加入到试管中,制备5%胆碱水溶液。使用JEIO TECH MC-11多搅拌器在40℃±0.1℃下将该水溶液搅拌2小时。In order to determine the in vitro stability of each double-coated choline prepared in Test Examples 1-15, each prepared ruminant-protected choline was placed in a test tube, and distilled water was added to the test tube to prepare 5% choline aqueous solution. The aqueous solution was stirred at 40°C ± 0.1°C for 2 hours using a JEIO TECH MC-11 multi-stirrer.

将搅拌的水溶液通过3号Whatman纸过滤以便仅仅收集固体。固体在45℃±0.1℃下至少干燥12小时以完全除去残余的水分。The stirred aqueous solution was filtered through No. 3 Whatman paper to collect only the solids. The solids were dried at 45°C ± 0.1°C for at least 12 hours to completely remove residual moisture.

将干燥的样品在Sanpla Dry Keeper中冷却到室温,将300mg冷却的样品完全溶解在氯仿和乙醇(1:1v/v)混合溶剂中。使用5%K2CrO4作为指示剂以及溶液0.1N AgNO3作为滴定剂测定溶液中胆碱的含量。The dried sample was cooled to room temperature in a Sanpla Dry Keeper, and 300 mg of the cooled sample was completely dissolved in a mixed solvent of chloroform and ethanol (1:1 v/v). Use 5% K2CrO4 as indicator and solution 0.1N AgNO3 as titrant to determine the content of choline in the solution.

下表1中显示了测定结果。如表1中所示,根据多孔板的孔尺寸的变化的体外胆碱损失变化很小或者没有变化(测试例1-4)。The measurement results are shown in Table 1 below. As shown in Table 1, there was little or no change in in vitro choline loss according to changes in the well size of the multiwell plate (Test Examples 1-4).

关于第一次封装材料的种类,与使用吐温80或者Span80的情况相比,在使用单价脂肪酸或者二价脂肪酸PEG作为第一次封装材料的情况下显示胆碱的体外损失减少。结果,可以观察到与使用单价脂肪酸、二价脂肪酸PEG、吐温80或者Span80相比,液体氢化油用作第一次封装材料能够导致胆碱的体外损失减少(测试例5-8)。Regarding the type of primary encapsulating material, compared with the case of using Tween 80 or Span80, the in vitro loss of choline was shown to be reduced when monovalent fatty acid or divalent fatty acid PEG was used as the primary encapsulating material. As a result, it was observed that the use of liquid hydrogenated oil as the primary encapsulation material resulted in reduced loss of choline in vitro compared to the use of monovalent fatty acid, divalent fatty acid PEG, Tween 80 or Span80 (Test Examples 5-8).

关于加入的第二次封装材料的量,可以看出所加入的第二次封装材料的量的增加可使胆碱的体外损失减少(测试例9-13)。With regard to the amount of secondary encapsulating material added, it can be seen that an increase in the amount of secondary encapsulating material added leads to a decrease in in vitro loss of choline (Test Examples 9-13).

而且,关于第一次封装材料与胆碱之比,可以观察到第一次封装材料与胆碱之比增加可使胆碱的体外损失减少(测试例14和15)。Furthermore, with regard to the ratio of primary encapsulating material to choline, it was observed that an increase in the ratio of primary encapsulating material to choline resulted in a decrease in the loss of choline in vitro (test examples 14 and 15).

表1Table 1

  测试例 体外损失(%) 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 test case In vitro 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

结果,可以发现,通过选择液体氢化油作为第一次封装材料,将胆碱与第一次封装材料以1:0.5或者1:1的比例混合,将混合物进行第一次封装步骤并使用曾家量的第二次封装材料将第一次封装的材料进行第二次封装步骤所制备的双涂层反刍保护的胆碱显示使体外损失降低到最小。As a result, it can be found that by selecting liquid hydrogenated oil as the first encapsulation material, mixing choline with the first encapsulation material at a ratio of 1:0.5 or 1:1, subjecting the mixture to the first encapsulation step and using Zeng's Quantities of secondary encapsulation material The double-coated ruminant-protected choline prepared by subjecting the first encapsulation material to a second encapsulation step was shown to minimize in vitro loss.

实施例3:反刍保护的胆碱的喂养测试Example 3: Feeding Test of Choline for Rumination Protection

对测试例15中制备的反刍保护的胆碱进行体内喂养测试,该胆碱在实施例2的测试中显示低体外损失并具有合适大小和高胆碱含量。In vivo feeding tests were performed on the rumination-protected choline prepared in Test Example 15, which showed low in vitro loss in the test of Example 2 and had a suitable size and high choline content.

为了使用反刍保护的胆碱进行奶牛喂养测试,选择处于中间哺乳期的10头奶牛作为测试动物并共给足够量的复合饲料的总混合定量,并且以12小时为间隔每天大量喂养2次。而且,当喂养总混合定量时反刍保护的胆碱(胆碱含量为25%)以每头母牛40g的量(以10g胆碱为基础)额外喂养母牛。母牛每天泌乳两次并且测定产奶量。从所产的奶中取得牛奶样品,并且使用自动分析仪(LactoScopeR,MK2,DeltaInstruments,The Netherlands)测定牛奶成分和牛奶样品中的体细胞数。For the dairy cow feeding test using rumination-protected choline, 10 cows in the middle lactation period were selected as test animals and given a total mixed ration of a sufficient amount of the compound feed and fed heavily twice a day at 12-hour intervals. Furthermore, rumination-protected choline (25% choline content) was additionally fed to the cows in an amount of 40 g per cow (based on 10 g choline) when fed the total mixed ration. Cows were lactated twice daily and milk production was measured. Milk samples were taken from produced milk, and the milk composition and somatic cell number in the milk samples were determined using an automatic analyzer (LactoScopeR, MK2, DeltaInstruments, The Netherlands).

测定结果在下表2中显示。如表2中所示,在其中将反刍保护的胆碱喂养给母牛的情况下,母牛的日牛奶产量从喂养前的29.2kg增加到喂养后的32.1kg,增加了9.9%,奶脂、奶蛋白、乳糖和总固体也分别增加了7.9%,10.4%,12.7%和10.1%。而且,由于喂养了反刍保护的胆碱,样品中体细胞数下降了61.9%,从167,000细胞/ml下降到103,000细胞/ml,表明反刍保护的胆碱在改善牛奶质量方面是有效的。另外,样品中胆碱含量的总量比对照增加了大约48.8%,从44.85mg/ml增加到66.75mg/ml,表明反刍保护的胆碱使其能够产生富胆碱牛奶。The measurement results are shown in Table 2 below. As shown in Table 2, in the case where rumination-protected choline was fed to the cow, the daily milk production of the cow increased by 9.9% from 29.2 kg before feeding to 32.1 kg after feeding, milk fat , milk protein, lactose and total solids also increased by 7.9%, 10.4%, 12.7% and 10.1%, respectively. Moreover, the number of somatic cells in the samples decreased by 61.9% from 167,000 cells/ml to 103,000 cells/ml due to feeding with rumination-protected choline, indicating that rumination-protected choline is effective in improving milk quality. In addition, the total amount of choline content in the samples increased by approximately 48.8% over the control, from 44.85 mg/ml to 66.75 mg/ml, indicating that rumination-protected choline enables the production of choline-enriched milk.

表2Table 2

  牛奶产量(kg/天) 奶脂 奶蛋白 乳糖 总固体 体细胞数(103/me) 胆碱(mg/me) 喂养前 29.2 3.43% 2.79% 4.49% 11.57% 167 44.85 喂养后 32.1 3.70% 3.08% 5.06% 12.74% 103 66.75 Milk production (kg/day) Creamy milk protein lactose total solids Somatic cell number (10 3 /me) Choline (mg/me) before feeding 29.2 3.43% 2.79% 4.49% 11.57% 167 44.85 after feeding 32.1 3.70% 3.08% 5.06% 12.74% 103 66.75

  含量变化 109.9% 107.9% 110.4% 112.7% 110.1% 61.9% 148.8% content change 109.9% 107.9% 110.4% 112.7% 110.1% 61.9% 148.8%

工业实用性Industrial Applicability

如上面详细描述的那样,本发明提供了一种制备双涂层反刍保护的胆碱的方法。根据本发明制备的反刍保护的胆碱不被瘤胃中的微生物、pH和水降解,从而可稳定地输送到下部消化道中并在其中被吸收。而且,当其被用于饲养反刍家畜时,其可增加反刍家畜对养分的利用,从而可使家畜产量增加,使其能够产生产生富胆碱牛奶的功能家畜。此外,本发明的用于制备反刍保护的胆碱的方法可用于保护各种成分不被反刍降解,并可用于各种新饲料添加剂的生产。As described in detail above, the present invention provides a process for the preparation of double-coated ruminant protected choline. The ruminant-protected choline prepared according to the present invention is not degraded by microorganisms, pH and water in the rumen, and thus can be stably delivered to and absorbed in the lower digestive tract. Also, when it is used to feed ruminant livestock, it can increase the utilization of nutrients by ruminant livestock, thereby increasing the yield of livestock, making it possible to produce functional livestock that produce choline-rich milk. In addition, the method for preparing rumination-protected choline of the present invention can be used to protect various components from being degraded by rumination, and can be used in the production of various new feed additives.

虽然已经参照特定特征对本发明进行了详细描述,但对本领域技术人员来说显而易见的是,该描述仅仅用于优选实施方式,而不是限制本发明的范围。因此,本发明的实际范围将由所付的权利要求书及其等同物来限定。Although the invention has been described in detail with reference to specific features, it will be apparent to those skilled in the art that the description is for the preferred embodiment only and does not limit the scope of the invention. Therefore, the actual scope of the present invention will be defined by the appended claims and their equivalents.

Claims (16)

1. method for preparing the ruminally protected choline of two coatings, this method comprises the following steps:
(a) from fixing choline, remove moisture on the carrier then and prepare the fixing choline of carrier through the liquid choline that concentrates is fixed on;
(b) choline that bonding agent/coating material and carrier is fixing mixes in blender and stirs, and encapsulation prepares the encapsulated choline first time in the extruding machine then;
(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 choline that the two coatings of preparation according to claim 1 are ruminally protected; 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 choline that the two coatings of preparation according to claim 1 are ruminally protected is characterized in that carrier is the water insoluble carrier that is selected from down group, and its group comprises silicon, cellulose, starch and zeolite.
4. the method for the choline that the two coatings of preparation according to claim 1 are ruminally protected; 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 the aliphatic acid with the fusing point that is higher than 40 ℃.
5. the method for the choline that the two coatings of preparation according to claim 4 are ruminally protected is characterized in that unit price soap is sodium soap or aliphatic acid potassium.
6. the method for the choline that the two coatings of preparation according to claim 4 are ruminally protected is characterized in that, at least a during divalence soap is selected from down and organizes, and its group comprises surfactant, calcium stearate, zinc stearate and dolomol.
7. the method for the choline that the two coatings of preparation according to claim 4 are ruminally protected 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 choline that the two coatings of preparation according to claim 1 are ruminally protected; It is characterized in that; The oil of said 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 choline that the two coatings of preparation according to claim 1 are ruminally protected is characterized in that said choline and said binding agent/coating material are with 1: the weight ratio of 0.1-2.0 is mixed with each other.
10. the method for the choline that the two coatings of preparation according to claim 1 are ruminally protected is characterized in that blender is selected from down group, and its group comprises ribbon mixer, agitator, homogenizer and V-type blender.
11. the method for the choline that the two coatings of preparation according to claim 1 are ruminally protected is characterized in that the extruding machine is an extruder.
12. the method for the choline that the two coatings of preparation according to claim 1 are ruminally protected is characterized in that the choline of encapsulation is graininess or needle-like for the first time.
13. the method according to the ruminally protected choline of the two coatings of claim 1 or 11 described preparations is characterized in that the porous plate in the said extruding machine is of a size of 0.5-2.5mm.
14. the method for the choline that the two coatings of preparation according to claim 11 are ruminally protected is characterized in that the temperature of the recipient in the said extruder remains on 10-60 ℃.
15. the method for the choline that the two coatings of preparation according to claim 1 are ruminally protected; It is characterized in that; Step (d) is carried out through the packaging system second time that is selected from down group, comprises super mixer, ribbon mixer, ROEDIGE blender and fluid bed processor.
16. the method for the choline that the two coatings of preparation according to claim 1 are ruminally protected is characterized in that two coating levels are 15-55% (w/w).
CN2006800544697A 2006-05-02 2006-11-14 Method for preparing ruminally protected choline Expired - Fee Related CN101431903B (en)

Applications Claiming Priority (4)

Application Number Priority Date Filing Date Title
KR1020060039733 2006-05-02
KR1020060039733A KR100698452B1 (en) 2006-05-02 2006-05-02 Method of preparing ruminant protective choline
KR10-2006-0039733 2006-05-02
PCT/KR2006/004773 WO2007126191A1 (en) 2006-05-02 2006-11-14 Method for preparing ruminally protected choline

Publications (2)

Publication Number Publication Date
CN101431903A CN101431903A (en) 2009-05-13
CN101431903B true CN101431903B (en) 2012-06-13

Family

ID=38655688

Family Applications (1)

Application Number Title Priority Date Filing Date
CN2006800544697A Expired - Fee Related CN101431903B (en) 2006-05-02 2006-11-14 Method for preparing ruminally protected choline

Country Status (4)

Country Link
JP (1) JP5159766B2 (en)
KR (1) KR100698452B1 (en)
CN (1) CN101431903B (en)
WO (1) WO2007126191A1 (en)

Families Citing this family (16)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US7955418B2 (en) 2005-09-12 2011-06-07 Abela Pharmaceuticals, Inc. Systems for removing dimethyl sulfoxide (DMSO) or related compounds or odors associated with same
WO2007033180A1 (en) 2005-09-12 2007-03-22 Abela Pharmaceuticals, Inc. Materials for facilitating administration of dimethyl sulfoxide (dmso) and related compounds
EP2324838A1 (en) 2005-09-12 2011-05-25 Abela Pharmaceuticals, Inc. Compositions Comprising Dimethyl Sulfoxide (DMSO)
KR101069118B1 (en) 2008-10-22 2011-09-30 경상대학교산학협력단 Method for preparing enteric choline chloride and choline chloride prepared according to the method
AU2010239355B2 (en) * 2009-04-23 2014-02-13 H.J. Baker & Bro., Inc. Granular feed supplement
CN101897463A (en) * 2009-06-01 2010-12-01 王中心 Method for producing ruminant rumen bypass product
MX353712B (en) 2009-10-30 2018-01-24 Abela Pharmaceuticals Inc Dimethyl sulfoxide (dmso) and methylsulfonylmethane (msm) formulations to treat osteoarthritis.
KR101219740B1 (en) 2010-06-07 2013-01-11 대한민국 Manufacturing method of Ruminally Protected Choline for high choline milk production And Ruminally Protected Choline Using Thereof
CN103549153A (en) * 2013-11-11 2014-02-05 张维 Rumen protected choline chloride particle as well as production method thereof
WO2015115618A1 (en) 2014-01-31 2015-08-06 森下仁丹株式会社 Orally administered agent for ruminants and ruminant feed containing same
CN104719670B (en) * 2015-03-24 2018-04-27 河北碧隆化工科技有限公司 A kind of high-content ruminant rumen choline chloride particle and preparation method thereof
CN104872395B (en) * 2015-06-05 2018-06-19 西双版纳华坤生物科技有限责任公司 A kind of milk and its production method rich in omega-fatty acid and conjugated linoleic acid
CN105166413A (en) * 2015-10-10 2015-12-23 山西农业大学 Rumen-bypass riboflavin additive for beef cattle and preparation method of rumen-bypass riboflavin additive
CN114423298A (en) * 2019-09-26 2022-04-29 味之素株式会社 Feed additive composition for ruminants
CN112167165B (en) * 2020-09-29 2022-02-11 厦门汇盛生物有限公司 Preparation and application of compound rumen-bypass polyunsaturated fatty acid powder
CN113331306A (en) * 2021-06-03 2021-09-03 北京中科万联科技有限公司 Additive for improving livestock and poultry physiological function based on yucca, and preparation method and application thereof

Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4948589A (en) * 1988-12-29 1990-08-14 Showa Denko Kabushiki Kaisha Granular composition for ruminant
WO1994015480A1 (en) * 1992-12-30 1994-07-21 Morgan Manufacturing Co., Inc. Composition and method for ruminant milk production
US5807594A (en) * 1997-02-26 1998-09-15 Ducoa, L.P. Method for enhancing feed efficiency in ruminants with an encapsulating choline composition
EP0781100B1 (en) * 1994-09-16 2000-07-19 Air Products And Chemicals, Inc. Animal feedstuffs and additives
EP1381285A1 (en) * 2001-04-16 2004-01-21 Jubilant Organosys Limited A rumen bypass composition containing a bioactive substance and a method for its preparation
CN1561979A (en) * 2004-04-21 2005-01-12 浙江大学 Micro capsule for choline chloride for ruminant stomach and its preparing method
CN1700912A (en) * 2002-09-24 2005-11-23 巴斯福股份公司 Choline ascorbate formulations

Family Cites Families (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4713245A (en) * 1984-06-04 1987-12-15 Mitsui Toatsu Chemicals, Incorporated Granule containing physiologically-active substance, method for preparing same and use thereof
BR8506634A (en) * 1984-12-20 1986-09-09 Rhone Poulenc Sante COMPOSITES FOR COATING FOOD ADDITIVES INTENDED FOR RUMINANTS AND GRANULATES IN THE FORM OF MICROCAPSULES SO COATED
US5190775A (en) * 1991-05-29 1993-03-02 Balchem Corporation Encapsulated bioactive substances
JPH06339343A (en) * 1993-04-08 1994-12-13 Ajinomoto Co Inc Feed additive for ruminant
JPH0764547A (en) * 1993-08-30 1995-03-10 Roland Corp Marker quantizer
JPH0787900A (en) * 1993-09-27 1995-04-04 Ajinomoto Co Inc Feed additive composition for ruminant
JPH08336360A (en) * 1995-03-17 1996-12-24 Kanagawa Kagaku Kenkyusho:Kk Feed composition for ruminant and feeding using the same
KR0163831B1 (en) * 1995-03-18 1998-11-16 비비바흐, 카르그 Method for preparing lysine protected against degradation in rumen and animal feed including the same
US6797291B2 (en) * 2002-01-09 2004-09-28 Balchem Corporation Stable hygroscopic compositions and methods for stabilizing hygroscopic ingredients

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4948589A (en) * 1988-12-29 1990-08-14 Showa Denko Kabushiki Kaisha Granular composition for ruminant
WO1994015480A1 (en) * 1992-12-30 1994-07-21 Morgan Manufacturing Co., Inc. Composition and method for ruminant milk production
EP0781100B1 (en) * 1994-09-16 2000-07-19 Air Products And Chemicals, Inc. Animal feedstuffs and additives
US5807594A (en) * 1997-02-26 1998-09-15 Ducoa, L.P. Method for enhancing feed efficiency in ruminants with an encapsulating choline composition
EP1381285A1 (en) * 2001-04-16 2004-01-21 Jubilant Organosys Limited A rumen bypass composition containing a bioactive substance and a method for its preparation
CN1700912A (en) * 2002-09-24 2005-11-23 巴斯福股份公司 Choline ascorbate formulations
CN1561979A (en) * 2004-04-21 2005-01-12 浙江大学 Micro capsule for choline chloride for ruminant stomach and its preparing method

Also Published As

Publication number Publication date
KR100698452B1 (en) 2007-03-23
JP5159766B2 (en) 2013-03-13
WO2007126191A1 (en) 2007-11-08
JP2009535056A (en) 2009-10-01
CN101431903A (en) 2009-05-13

Similar Documents

Publication Publication Date Title
CN101431903B (en) Method for preparing ruminally protected choline
JP7593808B2 (en) Process for producing encapsulated amino acids for ruminants
JP3448936B2 (en) Methods for increasing milk production in ruminants
KR20150039823A (en) Method of protecting active ingredient from degradation during pelleting
WO2020073800A1 (en) Rumen protected choline chloride microcapsule and preparatin method thereof
EP3206508A1 (en) Compositions for multiphased, staggered, or sustained release of an active substance
CN101467592A (en) Ruminant feed additive for protecting vitamin C and preparation method and application thereof
CN109843079A (en) Feed additive composition for ruminants
US20240165042A1 (en) Composition for controlled release of physiologically active substances and process for its preparation
JP7423999B2 (en) Feed composition, coated particles, method for producing feed composition
KR101219740B1 (en) Manufacturing method of Ruminally Protected Choline for high choline milk production And Ruminally Protected Choline Using Thereof
JPS61195653A (en) Particle for ruminant
US20220211076A1 (en) Additive composition for ruminant feeds
US11083209B2 (en) Feed additive composition for ruminants
JPH02163043A (en) Feed additive for ruminant
JPH0387151A (en) Feed additive for ruminant
JP2847882B2 (en) Ruminant feed additives
WO2020254678A1 (en) Feed additive
CA2862398A1 (en) A high energy rumen inert feedstuff

Legal Events

Date Code Title Description
C06 Publication
PB01 Publication
C10 Entry into substantive examination
SE01 Entry into force of request for substantive examination
C14 Grant of patent or utility model
GR01 Patent grant
CF01 Termination of patent right due to non-payment of annual fee
CF01 Termination of patent right due to non-payment of annual fee

Granted publication date: 20120613

Termination date: 20211114