DE1492905C - Colored vitamin preparation for use as a feed supplement - Google Patents

Description

In animal breeding, especially in poultry farming, feed has been used for a long time administered that are fortified with vitamins. You can use the animal feed in dry state with also dry vitamin preparations, which are known in various forms are, mix.

Such preparations are described, inter alia, in British patents 681 930 and 681 931, the USA. - Patent documents 2 933 392, 2 937 091, 973 266 and 2 940 900, the Hungarian patent specification 149 547 and the German Auslegeschrift 012 156. The known products represent granules in which the individual particles that contain the fat-soluble vitamin are mostly digestible Have a shell made of protein, vegetable gums, carbohydrates, waxes or similar substances or Are flakes obtained by drying a dispersion or emulsion of the vitamins in water.

The commercially available supplementary feed containing vitamins is usually added to the feed by the consumer mixed in. They should therefore not only be stable in storage, but also their even distribution and their Concentration in the feed must also be quickly and reliably recognizable for the layperson, otherwise the There is a risk of overdosing at least in places or the effect is impaired, "because that Animal does not receive enough vitamins.

It is already known to color vitamins to determine their presence and, if necessary, their concentration to be able to detect in the feed (USA patents 2,685,517 and 2,868,644). But since the colored vitamin pellets are so small that they cannot be easily recognized in the feed this method is not satisfactory. To determine the presence of vitamins in a feed therefore a sample of the latter has to be cumbersome, e.g. B. with the help of strongly magnifying lenses or by Removal of the vitamin pellets from the feed (as is known from US Pat. No. 2,685,517) to be analyzed.

Various methods of increasing the size of the vitamin particles have also been proposed, what but hardly succeeds without at the same time increasing the effective amount of vitamins in the individual particles.

In the production of animal feed fortified with vitamins with a certain vitamin content, if particles with a high vitamin content are used, fewer individual particles would have to be added, but this makes uniform distribution in the feed more difficult, since the particles with a high vitamin content are separated in the feed. There is also the risk of overdosing when using vitamin particles with a high vitamin content. Surprisingly, it has now been found that by mixing a non-toxic dye with a fat-soluble vitamin (preferably vitamins A and D), a water-soluble dextrin and an edible antioxidant, colored particles can be obtained in which the vitamins are more stable and which are easily visible in animal feed can be recognized without the vitamin-containing particles having to be removed from the feed or complicated analytical procedures having to be carried out.
In this way one can produce a vitamin-fortified feedstuff with a given vitamin content, in which the vitamin particles can easily be recognized. If colored vitamin-containing particles are produced in such a way that each color indicates the presence of a different vitamin, the presence of such differently colored vitamin particles in the feed can be determined with the naked eye. By adding the vitamin preparations according to the invention, a vitamin-fortified feed is obtained in which the vitamins are easier to use and more biologically effective than in the previously known vitamin-fortified supplementary feed.

The colored vitamin preparation according to the invention in the form of solid flaky particles with a content of one or more fat-soluble vitamins and possibly an edible one Antioxidant for use as a feed supplement is therefore characterized by a content of 70 to 95 weight percent water soluble dextrin, 0.1 to 5 weight percent non-toxic dye and optionally 0.1 to 5.0 percent by weight of an edible antioxidant, the flaky particles are so large that they pass a sieve with a mesh size of 0.84 mm and a sieve be retained with 0.074 mm clear mesh size.

In the vitamin preparation according to the invention, the water-soluble dextrin acts as a binding green mass with a softening effect, so that separate

small areas with a high vitamin content in the form of thin leaflets of high bulk density over the individual particles are distributed. This creates a multitude of colored, vitamin-containing particles in flake form with a correspondingly large surface area instead of the well-known pellets or pearls, which are a . have a certain area with high vitamin content and density. Furthermore, the dextrin distributes the non-toxic dyes and makes their color more vivid, so that all "parts of each flake are uniform." are colored and you get flakes of a certain color that are easy to spot in the feed are.

The dextrins contained in the vitamin preparations according to the invention together with the coloring agents are known and are derived from different strengths, e.g. B. corn, potato, tapioca, wheat, Sago, rice, soybeans, corn, etc. starch, if you add acids, enzymes, alkalis to the starch or treated by pyrolytic processes.

The preparation of the colored vitamin preparations according to the invention is carried out by homogeneously distributing \ a solution of at least one liposoluble Vit ^k amine, optionally with the addition of an edible antioxidant in an aqueous liquid at an elevated temperature, evaporation of the thus obtained liquid mass in a thin layer and crushing of the dry residue, and the production process according to the invention is characterized in that a solution of 70 to 95 percent by weight of a water-soluble dextrin, 0.1 to 5 percent by weight of a non-toxic dye and optionally 0.1 to 5.0 percent by weight of an edible antioxidant, based on the Particle weight, is used and the dry residue is broken up into flaky particles which pass a sieve of 0.84 mm clear mesh size and are retained by a sieve of 0.074 mm clear mesh size.

The vitamin can be a natural or synthetic fat-soluble vitamin, e.g. B. Vitamin A, Vitamin Use D, vitamin E or vitamin K or mixtures thereof. Activated sterols, e.g. B. Ergosterol Λ or irradiated 7-dehydro-cholesterol, vitamin A- ' Alcohol, synthetically produced vitamin A, fish oils, fish liver oils, vitamin concentrates made from such oils etc. are also suitable for the production of the preparations according to the invention. Furthermore can Vitamin A esters, e.g. B. Vitamin A acetate and vitamin A palmitate or precursors of vitamin A, e.g. Carotene, can be used. The vitamin source should preferably have a vitamin content of have about 20,000 to 3,000,000 U.S. Pharmacopoeia Units or more, with vitamin contents of about 100,000 to 600,000 U.S. units per gram are preferred. ·,

Any of the usual antioxidants can be used for the vitamin preparation according to the invention are, as far as it is edible, z. B. propyl gallate, butylated hydroxyanisoles, ethoxydihydrotrimethylquinoline, butylated hydroxytoluene, gallic acid, nordihydroguajaretic acid, etc., are also suitable vitamins E, mixed tocopherols and natural antioxidants e.g. B. those in the U.S. patents 2,345,576, 2,345,578, 2,396,680, 2,396,681, 2,433,593, and 2,434,790. A mixture is preferred from ethoxydihydrotrimethylquinoline and butylated hydroxytoluene. Furthermore, one can use the antioxidants use in a mixture with compounds that act synergistically, such. B. lecithin, citric acid or Alkyl phosphates. Those contained in the vitamin preparation according to the invention or to be used for its production The amount of antioxidant, based on the weight of the vitamin-containing particles, is 0.1 to 5.0 percent by weight.

To those contained in the vitamin preparation according to the invention or to be used for its production non-toxic dyes include those from the "Food and Drug Administration" so-called »F. D. & C. «- dyes, E.g. F. D. & C.-Green 1 and 2, F. D. & C-Red 2, 3 and 4, F. D. & C-Yellow 5 and 6, F. D. & C-Violet 1, F. D. & C.-Blau 1 and 2 and others. The amount of dye is 0.1 to 5 percent by weight, preferably less than 2 percent by weight based on the particle weight. * 0.1 percent by weight non-toxic Dyes are particularly beneficial and already give a color that is found in complementary feed can be easily discovered.

The water-soluble dextrin has in the inventive Preparations have a stabilizing effect and protect the vitamins against oxidative decomposition from moist air and warmth during storage. If necessary, other customary stabilizers can also be used be added, e.g. B. soybean meal, corn flour, cotton or flaxseed meal, Corn flour, wheat flour or bran, oat flour, peanut flour, rice husk waste, etc.

In the preparation of the preparations according to the invention, the water-soluble one is the first. Dextrin in Dissolved water and the solution contains the fatty and vitamin-containing material (concentrate), the antioxidant and the dye added in any order. Any additional stabilizer used is also added to the dextrin solution. Conversely, you can mix the others beforehand Prepare ingredients except dextrin and add the dextrin solution to the mixture. >

In the mixture thus obtained, the ingredients are uniformly distributed. From the at elevated temperature liquid preparation, the water is then evaporated, so that solid, flaky particles are obtained, which the dextrin, the vitamin, the antioxidant and optionally the additional stabilizer in contain a state that could be called a frozen solid phase.

To produce the flakes from the liquid feed

. preparation is heated this, z to about 8O ⁰ C and passes it through a conventional homogenizer. B. an ultrasonic homogenizer. The homogenized, still liquid material can be air-dried in a thin layer on a double drum dryer. The two drums are heated, preferably with steam, so that the liquid mass boils when it comes into contact with the drums. After the water has evaporated, the dry material remains in the form of a cohesive thin layer on the drum, from which it is scraped off. The flake material is comminuted in a known manner to a size suitable for use as a feed supplement, namely to flakes which pass a sieve of 0.84 mm clear mesh size and are retained by a sieve of 0.074 mm clear mesh size.

The vitamin preparation according to the invention can be used as feed for poultry, but also for pigs, Horses, cows, sheep and other domestic animals can be used. Such vitamin-fortified feedstuffs should contain about 2200 to 110,000 units of fat-soluble vitamins per kilogram.

When using the colored vitamin preparations according to the invention, their presence in the ready mixed feed can easily be seen with the naked eye without the vitamin-containing particles the lining must be removed with the help of complicated separation processes. Also is the amount of particles each vitamin unit is much larger than with the well-known vitamin-containing supplementary feed, so that the vitamins be distributed more evenly over the entire feed. The vitamin preparations according to the invention are special constant, d. i.e. the vitamins are anti-oxidation, e.g. B. when storing in the heat, largely protected and also against the effects of minerals with which they .in the feed come into contact.

The invention is explained in more detail with reference to the examples, in which parts are parts by weight and percent Weight percent are.

B IS PIE 1

To produce a colored, vitamin A palmitate containing supplementary feed with a vitamin content of about 125 000 USP units per gram was first preparing a dextrin solution and it was stirred in 88.62 parts Maisstärkedextrin in 60 ml of water at 80 ⁰ C. The solution, which was kept at 60 ^° C., was added to 0.5 part of FD&C dye red 4, which dissolved.

By mixing 1.41 parts of ethoxydihydrotrimethylquinoline and 0.47 parts of butylated hydroxytoluene with 9 parts of vitamin A palmitate (1,500,000 units / g) with stirring in a nitrogen atmosphere at 45 ° C., a vitamin A palmitate mixture was prepared which at 60 ⁰ C was added to the dextrin solution and thoroughly mixed with it by stirring in a nitrogen atmosphere. After stirring for 10 minutes, the liquid obtained was homogenized in the homogenizer for a further 2 minutes, so that a smooth red-colored liquid was obtained which was dried overnight at room temperature. The dried material was obtained in the form of large red-colored flakes which were comminuted on sieves in such a way that they passed a sieve of 0.84 mm clear mesh size and were retained by a sieve of 0.074 mm clear mesh size. The product had a Vitarriin A palmitate content of about 125,000 US Pharmacopeia Units per gram.

B ice pie I 2

To produce a colored, vitamin AAcetat containing preparation with a vitamin content of about 250,000 USP units per gram was prepared by stirring 85.93 parts Maisstärkedextrin in 60 ml of water at 80 ° C, a dextrin, which was then kept at 60 ⁰ C whereupon 0.50 parts of FD&C Red 4 dye was dissolved therein.

To produce a vitamin A acetate concentrate, 1.7 parts of ethoxydihydrotrimethylquinoline were added and 0.56 parts of butylated hydroxytoluene with 11.31 parts of vitamin A acetate (2,387,000 u / g) Nitrogen mixed at 45 ° C. The vitamin A acetate mixture thus obtained was added to the dextrin solution at 60 ° C and thus thoroughly under nitrogen stirred. After stirring for about 10 minutes, the liquid became one for 2 minutes as in Example 1 red liquid homogenized, which was dried overnight at room temperature. The so obtained Flakes were comminuted as in Example 1. The preparation had a vitamin A content of about 250,000 U.S. units per gram.

Example 3

To produce a preparation of vitamin A palmitate and acetate-containing particles with about 350 000. E./g was prepared by stirring 80.43 parts Maisstärkedextrin in 60 ml of water at 80 ⁰ C, a dextrin, which after cooling to 60 ⁰ C 0.5 parts of soluble FD&C Red 4 dye was added.

By mixing 2.26 parts of ethoxydihydrotrimethylquinoline and 0.5 part of butylated hydroxytoluene with 13.93 parts of vitamin A acetate (2,387,000 U / g) and 2.38 parts of vitamin A palmitate (1,500,000 U. / g) under nitrogen at 45 ° C to obtain a vitamin a solution, which was stirred thoroughly at 60 ⁰ C under nitrogen with the dextrin and homogenized as above. The red-colored liquid was then dried overnight at room temperature and the flakes obtained were comminuted as in Examples 1 and 2. The preparation had a vitamin A content of approximately 350,000 US units per gram.

Eg game 4

To produce a preparation of colored, vitamin D-containing particles with a content of about 200 000 US units per gram was prepared as above from 92.05 parts Maisstärkedextrin and 60 ml of water at 8O ⁰ C a dextrin in which at 60 ° C 0.25 parts of FD&C Dye Blue 1 was dissolved. By mixing this solution with a mixture of 4.0 parts of butylated hydroxytoluene and 3.7 parts of vitamin D in vegetable oil (5,500,000 US units per gram) at 60 ° C and homogenizing the mixture as above, a smooth blue liquid was obtained. which was dried overnight at room temperature. The preparation was then granulated as above, so that the flakes, which had been added to the blue-colored halide particles from Examples 1, 2 and 3, passed a sieve of 0.84 mm clear mesh size, but were retained by a sieve of 0.074 mm clear mesh size became. The preparation had a vitamin D content of approximately 200,000 US units per gram.

Example 5

For the purpose of visual recognition of colored dextrin-containing vitamin particles according to the invention in Feed in the dry state was a certain amount of one with the colored vitamin preparation Enriched feed is sieved through a sieve of 0.42 mm clear mesh width. the The portion going through the sieve was then sieved through a sieve with a mesh size of 0.25 mm,

I 492

7 8

part of the vitamin-rich feed was left behind. Components:

The portion _{n,. ac} xyri "i, _n ," _mn

,. ,. ~, -. ... j. °. j ".,. Ground Milokorn οΟ, ϋ

was divided into eight samples, which were placed on round filters- _c . ",, ,, _{0 / D,.} · _{7 / ln}

. ,, ....,. ^ö ", T-vi. r soy flour, 44% protein 34.0

Small sheets of paper about 25 cm in diameter r ^ ä « _{,» iw r n} ^ i, »n _m » M Vn

Γ ^r,. j · !. c τ- ua ι u <. L. Steamed bone meal z, 0

brought and examined visually for color stains 5 lime 15

became. The observed color spots were _c ,,> Y '/ ,, [ _Λ ' _ς

, ... ,, Salt (NaCl) * ... 0.5

then paid. Vitamin premix *) 2.0

For the wet determination, that became the dry one

Determination used, the fortified feed- 6.8 kg of this feed were mechanically using

Medium-containing paper sheets folded across, so io 0.24 g of the red, dextrin and vitamin A palmitate

that the feed came inside. The paper-containing particles from Example 1 and 0.035 g of the

was then removed by spraying on particles completely containing dextrin and vitamin D.

moistened and pressed together by hand, so Example 4 mixed. The fortified feed

that the inner surface of the moist paper had a vitamin A content of 4400 U./kg and

colored particles emerged. The resulting 15 have a vitamin D content of 1100 U / kg. It was

Color spots were counted. as described above in dry and moist form

A feed was examined for the content of colored particles as follows,

Settlement used: the results are shown in Table I.

Table I.
Visual dry and wet determination of the colored particles in the feed

Dry determination counted particles, '■ · Moisture determination , counted spots, PmHp counted particles, counted particles, Total number counted spots, counted spots, Total number Red blue 41 Red blue 47 1 18th 23 ■ 44 23 24 50 2 19th 25th 65 23 27 57 3 32 33 46 19th 38 50 4th 22nd 24 56 27 23 59 5 27 29 47 33 " 26th 72 6th - 21 26th 62 38 34 73 7th 32 30th 73 40. 33 67 8th 37 36 54.3 32 35 "■ 59.4 average 26.0 28.3 29.4 30-, 0

45

Example 6
(Comparative example)

A. For comparison with the preparations according to the invention, colored supplementary feed was used, which were produced according to known processes and which contain the vitamin together with gelatine (instead of according to the invention contained dextrin).

The test of the animal feed produced analogously to Example 5 showed that the dyed according to the invention Vitamin preparations in the finished feed are about 30 times easier to recognize than those made using known methods produced gelatin-containing particles. They were also in the wet state during the examination Particles according to the invention are 4 times more visible than those produced by known processes. The after Colored vitamin preparations produced by known processes are therefore visible to the naked eye in animal feed much harder to see than those of the present invention.

B. To demonstrate the better stability of the vitamin preparations according to the invention, portions were added of every 0.454 kg of feed with the following composition a sufficient amount of the vitamin-containing Particles from Example 1, 2 and 3 were added. A gelatin-containing vitamin preparation would be used for comparison examined. '· ■ · "' '■

55

Components: weight percent

Ground Milokorn 52.25

44% soy flour 30.00

Tallow .... 4.00

Meat and bone scraps 4.00

Fish meal 3.00

Dried whey 2.00

Residue from molasses fermentation 2.00

Bone meal 1.25

Lime 1.00

Table salt 0.25

Premix of vitamins and

Trace minerals *) 0.25

The vitamin-fortified feed was each divided into 3 equal parts. Part was turned into one The drying cabinet was kept at 36.7 ° C and the second part was kept for 3 months at room temperature

60

*) The vitamin premix, which made up 2.0% of the feed, contained the following ingredients (the amount of the ingredients is based on 45.4kg feed): 200mg riboflavin, 500mg dl calcium pantothenate, 1200 mg niacin, 2000 mg choline chloride (to 100% iges related), 0.5 mg vitamin B ₁₂ , 40000-iE (ICU) vitamin D ₃ , 200 mg procaine penicillin and 10 mg magnesium sulfate.

*) Contains the complete requirement for trace minerals and vitamins, with the exception of vitamin A.

309 633/119

left to stand and the third part placed in a drying cabinet kept at 45 ° C. The drying cabinet with 36.7 ° C were after 1, 2 and 3 months, the drying cabinet with 45 ° C after 3 and

10

Samples taken 6 weeks and examined for vitamin content. The vitamin content of the at room temperature preserved part was determined after 3 months. The results are shown in Table II.

Table II

Stability of vitamin Α palmitate in the particles according to the invention in feed (Theoretical addition = 55,000 U./kg)

Vitamin supplement ■ Salary Stability at 36.7 2 months ³ C 3 months Stability 1 be 45.4 ° C Stability at Vitamin A Pal determination 47 100 44 100 space attempt mitate / dextrin at Ver 1 month (81%) 3 weeks 6 weeks temperature Vitamin A Acetate / search start 51 800 46 500 42 700 51 500 41200 3 months 1 Dextrin 54 200 (77%) (76%) 52 200 Vitamin a acetate 52,000 48 500 43,000 49 600 41000 (96%) 2 Palmitate / 55 700 (80%) (73%) 50 900 Dextrin 51 800 48 200 39 400 (91%) 3 Vitamin A Pal 53 800 43 600 39 400 (73%) 50 200 mitate / gelatin (75%) (94%) 45 600 45 400 35 300 Ver 52400 (70%) 45 200 same (86%)

As can be seen from Table II, the vitamin preparations according to the invention were more stable than those according to known methods using gelatin-made vitamin-containing particles.

C. To prove the better biological usability de.r vitamin preparations according to the invention in feed compared to the known methods were prepared for 6 servings of the feed supplement of the above composition Amounts of the vitamin preparations according to Examples 1 and 2 and a gelatin-containing comparative preparation added, that the feed had a vitamin content of 10 500 U / kg.

The experiments were carried out with one-day-old chickens, of which there were 7 in each group to 9 found. Each group was divided into 3 subgroups. The exam ran over 28 days, taking the chickens were in electrically heated breeding cells; Food and water were given ad libitum. The temperature of the growth cells was maintained at about 26-29 ° C. To the effect of the Position of the cage on biological response like this To keep it as low as possible, different subgroups of the same group were caged with different Positions brought. All test animals as well as the feed were taken at the beginning of the experiment weighed and all relevant data recorded at weekly intervals. The single rations for the test animals, a freshly mixed, large feed batch was used at the beginning of the experiment made without additive, which was blended for 20 minutes. To ensure complete stability of the To ensure vitamins in the premixed feed, the amount of feed was adjusted to be in 3 days was completely consumed, and in addition, the unused part of the feed was stored cold.

After 28 days, three chickens were randomly selected from each group and the animals' livers removed and examined for their vitamin content. The average vitamin content of the liver was taken as Considered criterion for the ability to store in the liver. The results of the investigations are listed in Table III.

Table III

Biological usability of vitamins from vitamin-containing particles with dextrin versus particles with gelatin. (Results after 4 weeks - chickens as test animals.)

Vitamin supplement supply increase Lining Total spoke spoke after
4 weeks amount per g
Weight vitamin
admission tion in
the liver tion in attempt in g increase (Units) (E. each
Liver) the liver,
% the Vitamin A palmitate / dextrin 10 573 U./kg up
taken Vitamin A Acetate / Dextrin 10 573 U./kg 434.8 1779 8185 3320 Vitamins 1 Vitamin A palmitate / gelatin 10 573 U./kg 439.2 1791 8304 3390 .40.6 2 435.7 1826 8419 3090 40.8 comparison 36.7

From the table it can be seen that the biological utilizability of the vitamins from the invention dextrin-containing vitamin preparations is greater than that from the gelatin-containing one used for comparison Vitamin supplement, because the percentage stored in the liver from the vitamin supplements Vitamins is significantly larger in the former case than in the known gelatin-containing vitamin preparations. Also the number of vitamin units each At the end of the experiment, the liver is in test animals fed with dextrin-containing vitamin preparations bigger than the others. This shows that the vitamins ingested by the test animals were superior Have effectiveness when the vitamins in preparations made according to the invention with dextrin are included.

Attention should also be drawn to the fact that the exploitation of the invention is subject to statutory provisions, in particular the Feed Act, may be restricted.

Claims (2)

Patent claims: 1. Colored vitamin preparation in the form of solid, flaky particles with a content one or more fat-soluble vitamins and possibly an edible antioxidant for use as feed supplement, characterized by a content of 70 to 95 weight percent water soluble dextrin, 0.1 to 5 weight percent non-toxic dye and optionally 0.1 to 5.0 percent by weight of an edible antioxidant, the flaky Particles are so large that they pass a sieve with a mesh size of 0.84 mm and be retained by a sieve with 0.074 mm clear mesh size. 2. A method for producing a colored vitamin preparation according to claim 1 by homogeneous Distributing a solution of at least one fat-soluble vitamin, optionally with an additive an edible antioxidant, in an aqueous liquid at elevated temperature, evaporation the resulting liquid mass in a thin layer and crushing the dry residue, characterized in that the aqueous liquid used is a solution of 70 to 95 percent by weight of a water-soluble dextrin, 0.1 to 5 percent by weight of a non-toxic dye and optionally 0.1 to 5.0 weight percent of an edible. Antioxidant, related based on the particle weight, and the dry residue is converted into flaky particles breaks, which pass a sieve of 0.84 mm clear mesh size and of a sieve of 0.074 mm clear mesh size are retained.