JP3266656B2 - Vitamin-impregnated granules and method for producing the same - Google Patents

Description

DETAILED DESCRIPTION OF THE INVENTION

[0001] The present invention relates to a vitamin-impregnated granule which is stabilized against oxygen, heat, light and the like, and in which individual particles are free from sticking and have high fluidity. Specifically, the present invention relates to a method for producing a water-dispersible or water-soluble granule containing a fat-soluble vitamin, a surfactant, and a saccharide porous granule, and a feed additive containing the granule.

[0002]

[Prior Art] "List of Standards of Ingredients for Feed Additives" issued by the Japan Society of Chemical Feedstuffs (4th edition, July 1, 1992)
1 day issued, supervised by the Ministry of Agriculture, Forestry and Fisheries, Livestock Division, Ministry of Agriculture, Forestry and Fisheries) Vitamin A powder is produced by powdering or coating and granulating "Vitamin A oil", retinol acetate or retinol palmitate with a suitable base. That the vitamin D powder is “cholecalciferol”, “ergocalciferol” or an edible vegetable oil solution or vitamin D ₃
It is manufactured by powdering or coating and granulating oil with a suitable base, and vitamin E powder is dl-α acetate.
It is described that tocopherol is produced by powdering or coating and granulating with a suitable base.
In addition, the document states that "vitamin A oil" includes caramel, wheat starch, rice bran oil cake, skim milk powder, white sugar, brewer's yeast,
Powdered vitamin A mixed with silicic anhydride or salts thereof
Formulation: Formulation of "Vitamin D powder" mixed with flour, rice bran oil cake, lactose, silicic anhydride or its salts, calcium hydrogen phosphate, etc .; "Vitamin D ₃ oil" with wheat starch, rice bran oil cake, skim milk powder , white sugar, vitamin D ₃ formulations powdery was admixed anhydrous silicic acid or its salts and the like; flour "vitamin E powder", rice bran oil cake, soybean cake, vitamin E formulations were mixed with anhydrous silicic acid or its salts and the like And "Vitamin A oil", "Vitamin A powder" or their preparations and "Cholecalciferol",
"Ergocalciferol", "vitamin D ₃ oil",
"Vitamin D powder" or a powdered vitamin AD preparation obtained by mixing these preparations with flour, rice bran oil cake, vegetable oil, soybean oil cake, animal oil, glucose, silicic anhydride or salts thereof, and "Vitamin A oil""VitaminA" powder ", or their formulations," cholecalciferol "," ergocalciferol "," vitamin D ₃ oil "," vitamin D powder "
Or these preparations and "dl-α-tocopherol acetate", "vitamin E powder" or these preparations are mixed with flour, rice bran oil grounds, vegetable oil, soybean oil grounds, animal oil, glucose, anhydrous silicic acid or salts thereof, etc. Powdered vitamin ADE preparations or vitamin-containing liquid preparations are also described.

Further, a method for producing a powder containing vitamin A in a form in which vitamin A is encapsulated in a dry solid of sugar is disclosed in JP-B-56-32291, and a coating agent such as vitamin, gelatin and sugar, triglyceride, and the like. A composition comprising a complexing agent and a complexing agent is also described in JP-A-2-693. However, in the production process, a drying step is required because the components are dispersed in water and mixed. Moreover, the inventions described in the above publications aim at obtaining a stabilized composition of vitamin A, and do not disclose use as a feed additive.

[0004]

However, these known vitamin preparations are in the form of powders or liquids, which are inconvenient to handle, and have disadvantages in that their preparation is complicated.

[0005]

The present invention has succeeded in overcoming the above-mentioned disadvantages of the prior art by using a preformed porous saccharide granule as a material for supporting a vitamin in the present invention.

[0006]

The present invention SUMMARY OF THE INVENTION] has been impregnated with vitamins and surfactants, excellent saccharides porosity of fluidity with an apparent density of 0.55~0.82g / cm ³ and particle size 0.25~2.2mm Related to granular material. The granules are useful as feed additives.

Further, in the present invention, the vitamin and the surfactant are heated and stirred at a temperature lower than the decomposition temperature of the vitamin to form a uniform mixture, which is then formed into a preliminarily formed apparent density of 0.45 to 0.68 g / cm. ³ and particle size 0.25 to 2.2 mm
The vitamin is impregnated into the pores of the porous saccharide granules by uniformly mixing with the porous saccharide granules having the following formula:

The preformed porous saccharide granules usable in the present invention have an average particle size of 0.25 to 2.2.
mm and an apparent density of 0.45 to 0.68 g / cm ^3, preferably 0.49 to 0.67 g / cm ³ . And these sugars include sucrose, glucose, fructose,
There are oligosaccharides and starch hydrolysis products, and sucrose is particularly preferred. For example, Frost Sugar series (eg, Frost Sugar Standard, Frost Sugar OM. OMM type, etc.) manufactured by Nisshin Sugar Co., Ltd. can be used. . This frost sugar is granulated sugar, which has immediate solubility in water, solidification resistance, moisture absorption resistance, foaming properties, fragrance retention,
It is considered to be optimal for use in the present invention because it has properties such as heat resistance, soft sweetness due to pure sugar, and good mixing properties.

Unless otherwise specified, the term vitamin in the present invention means fat-soluble vitamin itself, its derivatives and precursors, such as vitamin A, its palmitate or acetate, vitamin E or its acetate, vitamin D (for example, D _2, D ₃ and its activated form), vitamin K, beta-carotene include ubiquinones like.

Examples of the surfactant include glycerin fatty acid ester (polyglycerin fatty acid ester), sorbitan fatty acid ester, polyoxyethylene sorbitan fatty acid ester and polyoxyethylene glycerin fatty acid ester (including polyoxyethylene castor oil and hardened castor oil). Species or two or more species can be used. Examples of the glycerin fatty acid ester include NIKKOL DGMO-C (diglycerol monooleate) and DGDO (diglycerdioleate) of Nikko Chemicals Co., Ltd. Examples of sorbitan fatty acid esters include Kao
Emazole L-10 (F) (sorbitan monolaurate) manufactured by Nikko Chemicals Co., Ltd. and NIKKOL SO-10R manufactured by Nikko Chemicals Co., Ltd.
(Sorbitan monooleate) and SO-15R (sorbitan sesquioleate). Examples of polyoxyethylene sorbitan fatty acid esters include NIKKOL TL-10 (POE (20) sorbitan monolaurate), TP-10 (POE (20) sorbitan monopalmitate) and TO-TO manufactured by Nikko Chemicals Co., Ltd. 10M (POE (20) sorbitan monooleate), TO-30 (POE (20) sorbitan trioleate),
There are TO-106 (POE (20) sorbitan monooleate) and TI-10 (POE (20) sorbitan monoisostearate). Examples of polyoxyethylene glycerin fatty acid esters include Cresphor EL (polyoxyethylene castor oil) manufactured by BASF, and NIKKOL CO-10 (POE (10) castor oil) and CO-40TX manufactured by Nikko Chemicals Co., Ltd. (POE
(40) Castor oil), CO-60TX (POE (60) castor oil), HC
O-5 (POE (5) hydrogenated castor oil), HCO-20 (POE (20) hydrogenated castor oil), HCO-40 (POE (40) hydrogenated castor oil), HCO-6
0 (POE (60) hydrogenated castor oil), HCO-80 (POE (80) hydrogenated castor oil) and HCO-100 (POE (100) hydrogenated castor oil).

In the present invention, the saccharide porous granular material as described above is used, and this is impregnated with a vitamin and a surfactant.
Vitamin is impregnated in the pores of the saccharide porous granules and hardly adheres to the surface. This is presumed from the fact that the apparent density of the raw material saccharide particles is 0.45 to 0.68 g / cm ³ , whereas the apparent density of the granular material is 0.55 to 0.82 g / cm ^3. . Therefore, the granular material obtained by the method of the present invention has excellent fluidity and is convenient for handling.

The above-mentioned surfactant acts as a solubilizer or dispersant for solubilizing or dispersing the vitamin, and when the mixture of the vitamin and the surfactant is mixed with the saccharide porous granular material, the surfactant is added. The saccharide porous granules can be uniformly impregnated into the saccharide porous granules, and when the saccharide porous granules thus impregnated with the vitamins coexist with water, the vitamins can be impregnated in water. It also acts as a solubilizer or emulsifier.

In a preferred embodiment of the present invention, the present granules can further contain a conventional antioxidant.
These antioxidants include, for example, dibutylhydroxytoluene, butylhydroxyanisole and ethoxyquin. In addition, water-soluble vitamins, for example, vitamins B, vitamin C, and the like can be included in the present granular material alone or in combination of several types.

The proportion of the vitamin, surfactant and saccharide porous granules to be present in the granules obtained in the present invention can vary depending on the specific examples of each component used, but generally, the proportion of vitamins based on the total weight is If it is 22% by weight or less, it can be sufficiently impregnated, and the surfactant should be as small as possible, but preferably about 3 to 25% by weight.

In the granular material of the present invention, in addition to the above-mentioned components, well-known additives usually used in the fields of feed, food and medicine, for example, stabilizers, lubricants, disintegrants, preservatives・ Sweetening agents, flavoring agents, coloring agents, etc. can be added.

The granules of the present invention are usually prepared by heating and stirring a vitamin and a surfactant at a temperature of about 40 ° C. to a temperature lower than the decomposition temperature of the vitamin to form a uniform mixture, and mixing the mixture with the porous saccharide granules at room temperature. Produced by mixing homogeneously in a mixer at ~ 70 ° C. At this time, a small amount of an organic solvent such as ethanol, acetone or the like can be added as a diluent in order to facilitate mixing of the vitamin and the surfactant or penetration of the mixture into the porous saccharide granules. The mixer may be a conventional powder and liquid mixer, and for example, a Loedige mixer manufactured by Loedige may be used. The mixing temperature of the vitamin and the surfactant is preferably about 50 to about 70C, and the mixing of the mixture with the saccharide porous granules is preferably performed at about 50 to about 70C. In addition, the mixture of the mixture with the saccharide may be performed by adding the latter to the former, or may be performed by, for example, spraying the former into the latter. In this way, granules having a granular appearance and a smooth appearance and high fluidity are obtained. These can be stored for a long period of time in a cool storage at about 15 ° C., and there is no problem in stability.

Furthermore, in the production method of the present invention, by using the above-mentioned surfactant and saccharide porous granules as raw material components, high-speed stirring, which is an operation conventionally required in this kind of production technology, is carried out. Cooling and drying steps can be omitted and the effects such as simplification of the manufacturing process and improvement of the quality of the obtained granules and ease of handling are obtained.

According to still another feature of the present invention, a feed additive having excellent vitamin absorbability can be obtained by using the granules obtained by the present invention.

In recent years, the importance of vitamin A, D ₃ , and E supply to cattle has been emphasized, and various dosage forms of AD ₃ E agent have been used. However, there is a marked difference in the blood concentration of vitamins after administration depending on the dosage form of the liquid, powder or rumen bypass agent used so far. Due to the complicated administration of oral administration, frequent application to large numbers of animals is often inconvenient.

However, when the water-dispersible or water-soluble vitamin-containing granules according to the present invention are used, a remarkable vitamin-absorbing effect is achieved by natural feeding, and a stable feed additive which can be stored for a long period of time. Can be obtained.

The effect of vitamin absorption in cattle upon administration of the vitamin-impregnated granules obtained according to the present invention was examined. Test Example 1 As test cows, adult cattle of Holstein breeds weighing 601 kg to 790 kg and being 3 to 6 years old were divided into 5 groups, and 3 cattle in each group were used. As the vitamin-impregnated granules used in the test, those obtained by the following method were used.

[0022] Vitamin E acetate 111.1 g, vitamin A palmitate 17.4 g, vitamin D ₂ 0.10
7 g, 92.5 g of polyoxyethylene sorbitan monooleate (NIKKOL TO-10M manufactured by Nikko Chemicals Co., Ltd.),
The same operation as in Example 1 was performed using 10.1 g of BHT and 769 g of saccharide porous granules. The obtained granules have a smooth appearance and are rich in fluidity, and the granules contain 25,000 IU of vitamin A and vitamin D in 1 g.
₃ Impregnated with 2500 IU, 100 mg of vitamin E.

Further, for comparison, an experiment was conducted using a powdery agent shown by the following method.

Vitamin A coated with gelatin and sugar by spray drying (Lutabit A manufactured by Nisshin Birdish Co., Ltd.)
500), Vitamin D ₃ (Lutavit D ₃ 1000 manufactured by Nisshin Birdish Co., Ltd.) and Vitamin E impregnated in silicic acid (Lutabit E50 manufactured by Nisshin Birdish Co., Ltd.), and diluted and mixed with rice bran oil residue. A powder was obtained. This powder, like the above-mentioned granules, contains 25,000 vitamin A per gram.
0IU, vitamin D ₃ 2,500IU, vitamin E 100mg
Is contained.

Erythrocyte vitamin E was obtained by high performance liquid chromatography (vitamin, vol. 51, pp. 415-422, 197).
7 years), serum vitamin A palmitate was determined by high performance liquid chromatography (vitamin, vol. 53, pp. 358-35).
9, 1979).

Hereinafter, the results are shown in Tables 1 and 2.

[0027]

[Table 1]

[0028]

[Table 2]

Test Example 2 Six calves of the Holstein breed, 21 to 34 days old, weighing 43 to 54 kg, were divided into two groups, and the vitamin-impregnated granules and the powder were added in the same manner as in Test Example 1 at 0.05 g / kg BW. As a mixture with milk during feeding. Hereinafter, the results are shown in Tables 3 and 4.

[0030]

[Table 3]

[0031]

[Table 4]

From the above results, when the vitamin-impregnated granules according to the present invention were administered to adult cattle and calves by natural feeding and feeding, respectively, red blood cell vitamin E and serum vitamin A palmitate and calf after administration to adult cattle were obtained. The values of erythrocyte vitamin E and serum vitamin A palmitate after administration were clearly increased, and were extremely good compared to the powder administration used for comparison. Almost the same results were obtained.

Test Example 3 For comparison with the preparation (I) used in Test Example 1, a vitamin A preparation coated with gelatin and saccharides by a spray drying method (Lutabit A500 manufactured by Nisshin Birdish Co., Ltd .: (II)) Was used to conduct a stability test of vitamin A palmitate. Vitamin A palmitate was measured by the high performance liquid chromatograph method described above.

[0034]

[Table 5]

[0035]

[Table 6]

[0036]

The present invention will be described below with reference to examples and comparative examples, but the present invention is not limited to these examples.

Example 1 5 g of vitamin E acetate and 5 g of vitamin A palmitate and 13 g of polyoxyethylene sorbitan monooleate (NIKKOL TO-10M manufactured by Nikko Chemicals Co., Ltd.) were heated and mixed at about 60 ° C. On the other hand, saccharide porous granules (Frost Sugar Standard manufactured by Nisshin Sugar Co., Ltd .; particle size 0.85 mm, apparent density 0.49 g / cm) were placed in a mixer.
³ ) Charge 77 g, add the above mixture while mixing and mix for about 2 minutes to obtain a uniform granular product (particle size 0.8).
5 mm and an apparent density of 0.64 g / cm ³ ) were obtained. The product had a smooth appearance and was very fluid.

Example 2 214.9 g of vitamin E acetate, 344.8 g of vitamin A palmitate and 2.05 g of vitamin D ₃ and polyoxyethylene sorbitan monooleate (NIKKOL TO-10M manufactured by Nikko Chemicals Co., Ltd.) 0 g, polyoxyethylene sorbitan triolate (Nikko Chemicals Co., Ltd.)
NIKKOL TO-30) 314.4 g, polyoxyethylene castor oil (Cremophor EL manufactured by BASF) 207.
9 g, 45.5 g of sorbitan monolaurate (Emazole L-10 (F) manufactured by Kao Corporation) and 7.0 g of ethoxyquin
And 2.5 g of disodium hydrogen phosphate were heated and mixed at about 67 ° C. On the other hand, 425.0 g of Frost Sugar Standard was charged into a mixer, and the above mixture was added thereto while mixing, followed by mixing for about 2 minutes to obtain a uniform mixture (particle size: 0.85 mm, apparent density: 0.64 g / cm ^3). ) Got. The granular product was smooth and fluid. When a cross section of this product (a new cross section was formed by folding the granules) was taken using a scanning electron microscope, it was found that the above mixture was impregnated inside the porous saccharide granules.

Comparative Example The formulation described in Example 1 was repeated using lactose, granulated sugar and sucrose in place of the saccharide porous granules. The product was moist amorphous (nodular).

Example 3 Vitamin E acetate and polyoxyethylene sorbitan monooleate (NIKKOL TO-10M) were mixed with 3,
8, 13, 19 and 20.5 g with 20, 15, 10,
By heating and mixing at about 60 ° C. in the amounts of 4 and 2.5 g, five mixtures were prepared. On the other hand, 77 g of Frost Sugar Standard was charged into a mixer, and the above mixture was added thereto while mixing, followed by mixing for about 2 minutes to obtain five uniform products.

Also, vitamin E acetate 19 g, NIKK
OL TO-10M 2g, Gremphor EL 1.2g, NIKKOL TO-30
The above operation was repeated using 0.4 g, 0.4 g of Emazole L-10 (F) and 77 g of Frost Sugar Standard to obtain a uniform granular product.

The above product was subjected to a solubility test according to the following method. 1 g of the above product was weighed into a 100 ml transparent sample bottle, 100 ml of water was added thereto, and the bottle was capped. After the sample bottle was shaken well, it was left at room temperature, and its appearance was observed 24 hours later.

Among the above six products, in the case of a product using 20.5 g of vitamin E acetate, 2.5 g of NIKKOL TO-10M and 77 g of frost sugar standard, 2
After 4 hours, the oil had separated and oil and solids had floated. The remaining one was still uniformly emulsified even after 24 hours.

Example 4 Frost Sugar OMM (S) as Sugar Porous Granules
(Particle diameter 0.65 mm, apparent density 0.65 g / cm ³ ), Frost Sugar OMM (W) (particle diameter 0.28 mm, apparent density 0.2)
67 g / cm ³ ) or Frost Sugar OM (S) (particle size: 1.19 mm, apparent density: 0.65 g / cm ³ ), and when the formulation described in Example 1 was repeated, a smooth appearance was similarly obtained. Thus, granules having high fluidity (apparent density: 0.8 g / cm ³ ) were obtained.

Example 5 1.43 g of β-carotene was dissolved in 3.24 g of peanut oil by heating, and polyoxyethylene sorbitan monooleate (NIKKOL TO-10M manufactured by Nikko Chemicals Co., Ltd.) 15.3
3g, BHT 3.00g and saccharide porous granules (Nisshin Sugar Relost Sugar Standard) 77.0
The same operation as in Example 1 was performed using 0 g. The obtained granules had a smooth appearance and were rich in fluidity.

────────────────────────────────────────────────── ─── Continuation of the front page (72) Inventor Hiroshi Shibata 201-93 Nakano, Ueda-shi, Nagano Prefecture (56) References JP-A-3-86837 (JP, A) JP-B-56-32291 (JP, B1) Special Table 1986-501253 (JP, A) (58) Field surveyed (Int. Cl. ⁷ , DB name) A23K 1/00-1/20 A61K 9/00

Claims (3)

(57) [Claims] Claims: 1. A vitamin and a surfactant impregnated,
Apparent density 0.55-0.82 g / cm ³ and particle size 0.25
Excellent flowable saccharide porous granules having a size of about 2.2 mm. 2. The granular material according to claim 1, which is a feed additive. 3. Heating and stirring the vitamin and the surfactant at a temperature lower than the decomposition temperature of the vitamin to form a homogeneous mixture, which is then formed into a preformed apparent density of 0.45.
~0.68g / cm ³ and a manufacturing method of claim 1 granulate described which comprises uniformly mixing saccharides porous granules about 70 ° C. temperature below having a particle size 0.25～2.2Mm.