IL96899A

IL96899A - Compositions in the form of pellets containing active principles protected against degradation in the rumen of ruminants and process for their preparation

Info

Publication number: IL96899A
Application number: IL9689991A
Authority: IL
Original assignee: Rhone Poulenc Nutrition Amimal
Priority date: 1989-12-28
Filing date: 1991-01-07
Publication date: 1994-08-26
Also published as: IE904724A1; IE65337B1; MX173330B; HUT60902A; AU643722B2; KR0143766B1; MX23971A; NZ236685A; DK0437388T3; CZ280981B6; EP0437388A1; FR2656772A1; DE69101490D1; FR2656772B1; ES2062697T3; KR910014045A; AU6845090A; HU910040D0; DE69101490T2; CA2033234A1

Abstract

The present invention relates to novel compositions, in the form of pellets, used for the dietary and/or medicinal supplementation of ruminants, containing active substances protected against degradation in the rumen and one or more solubilisable, cross-linkable or meltable binders and, if appropriate, a separation agent and/or a filler.

Description

Ji nTm ti>*i*o:_>-i COMPOSITIONS IN THE FORM OF PELLETS CONTAINING ACTIVE PRINCIPLES PROTECTED AGAINST DEGRADATION IN THE RUMEN OF RUMINANTS AND PROCESS FOR THEIR PREPARATION The present invention relates to a process for the incorporation of active principles in pellets. It relates more especially to the incorporation in pellets of active principles protected against the enzymes of the rumen of ruminants. It relates still more especially to the preparation of pellets intended for incorporation in the feed of ruminants.

"Pellet" is understood to mean a nutrient granule for animals obtained either by extrusion of a feed mixture through a die or by another technique.

They take the form of sticks, preferably cylindrical, possessing, in particular, average sizes of 4 to 20 mm in length and 4 to 10 mm in diameter. They are widely used, since they are easy to handle and administer and are not dust-forming.

The problem which the present invention endeavours to solve consists in incorporating in "pellets" intended for animal feed granules containing compounds useful to their nutrition and/or to the therapy of these animals, but which cannot undergo pelletization on account of their sensitivity to temperature, pressure and shearing. In effect, pelletizing machines are machines which permit shaping by forcing a feed mixture through a die in the presence of steam.

This mixture is passed through a perforated plate (the die) by means of a press, which forces the mass to be extruded through the holes in the plate. On emerging from the die, the cylinders obtained are cut by a mechanical means or spontaneously. During the forced passage through the die, products having low thermal resistance or mechanical strength undergo degradation due both to the pressure exerted and to heat caused both by friction and by the addition of steam which promotes cohesion of the various floury ingredients of the base feeds.

This problem has already been raised in various earlier documents. Among these earlier documents, there may be mentioned the European patent application published under number EP 231,817, which describes a process for preparing "agglomerated feeds" based on vitamins or on compounds essential to human or animal health. It was known in the prior art that, when these compounds undergo a temperature rise during passage through pelletizing machines, they are at least partially destroyed. In effect, compounds having low thermal resistance or mechanical strength are often mixed, in order to shape them, with molasses, and undergo the action of steam in order to effect their cohesion. The simultaneous action of steam and pressure destroys them. Patent Application EP 231,817 enabled the problem of manufacture of these "agglomerated feeds" to be solved by spraying a solution or suspension of the vitamin or vitamins or the drug, and optionally a fat, onto a base core. This process permits only a coating of the base substanoe with the vitamin, with or without a fat. The said process is easy to carry out using pulverulent or liquid products such as vitamins or drugs. These products are thus easy to use in the form of a solution or suspension. The same does not apply when "agglomerated nutrient granules" are formed, in which the material sensitive to heat and/or compression itself takes the form of granules of average diameter approximately 0.3 to 5 mm, this being the case in the present invention.

In the French patent published under number FR 2,338,653, a process is also described for preparing feedingstuffs, onto which is sprayed an enzyme suspension, preferably of proteases, in a liquid or molten fat. This process provides the same teaching as the European application referred to above, and enables only "pellets" on which the temperature-sensitive substance is deposited at the periphery by a spraying phenomenon to be obtained.

The problem which the present invention has endeavoured to solve is to make additives which can be destroyed in the rumen of ruminants , such as amino acids, vitamins and also other nutritional or medicinal additives, into the form of "pellets" which are directly assimilable by the animals.

It is known, for example, that some amino acids are essential in the feeding of ruminants since they are limiting in the daily nutritional intake. This applies, in particular, to methionine and .lysine. These substances, when administered orally to ruminants, are destroyed in the rumen by the action of the digestive enzymes and microorganisms present in this organ. It has been discovered that, for these compounds to be utilizable by the animal and beneficial thereto, it was necessary to protect them with a substance enabling them to pass through the rumen without damage but capable of disintegration in or after the abomasum, so as to release the active substance in the intestine and thereby enable it to pass into the body.

In general, known coating compositions consist of a combination of a substance sensitive to pH variations, selected, in particular, from synthetic basic copolymers, with hydrophobic substances which may be selected, for example, from fatty acids or their derivatives and hydrophobic polymers. Such compositions are described, for example, in French Patents FR 78/23,966 (2,401,620), FR 78/23,968 (2,401,621) or FR 81/18,954 (2,514,261).

Among the main groups of coating agents, copolymers of vinylpyridine and styrene with a hydrophobic substance, preferably stearic acid and/or a non-water-soluble polymer, for example ethylcellulose, may be mentioned by way of examples.

The group of coating agents involving enzymatic digestion, such as chitosan and/or zein, combined with a hydrophobic substance, preferably stearic acid, and optionally a non-water-soluble polymer, preferably ethylcellulose, may also be mentioned.

The granules of protected active principles obtained take the form of more or less spherical particles having an average diameter of between 0.3 and 5 mm, and preferably approximately 2 mm.

It is inconceivable that granules of this size could be sprayed onto "pellets" of nutrient material. Neither can these granules be introduced into pelletizing machines, since the coating undergoes attack by phenomena such as abrasion, shearing, temperature rise, the addition of steam and pressure, which bring about an at least partial degradation of the coating and hence an instability of the active principles in the rumen on ingestion by the animal.

Hence it appeared to be impossible to make ruminants ingest the said protected active principles other than by dispersing the latter in the feed, which creates problems of homogeneity, concentration and distribution.

U.S. Patents Nos. 4,181,710, 4,181,708, 4,876,097 and 4,780,315 discloses compositions containing granular active principles protected against degradation in the rumen. The granular active principles have an average diameter of from about 0.3 to about 0.5 mm. When mixed with the cattle feed, these granules are too small to be consumed by the animal and, in addition, they are not mechanically stable when mixed with granular feed, due to the difference in size and form between the feed granules and these active principle granules . 5a In contrast, the present invention provides special pellets comprising active principle granules which are bound by a binding agent.

The special pellets of the invention are much larger than the active principle granules. These apecial pellets contain heat-sensitive substances and are manufactured by a special process which does not employ either heat or pessure.

The present invention has enabled this objective to be attained. It consists in preparing "special pellets" containing active principles protected against degradation in the rumen/ used for the nutritional and/or medicinal supplementation of ruminants, characterized in that they are obtained by mixing the protected active principle in granule form and a binding agent selected from binding agents capable of being solubilized, those capable of being crosslinked and binding agents capable of being melted, and optionally a disintegrating agent and/or a filler.

The active principles protected against the action of the rumen which are usable in this form are selected from: - essential amino acids, their salts, their derivatives and their analogues, such as: methionine lysine - vitamins - medicinal principles such as antibiotics.

The binding agents which are usable in the context of the present invention are preferably selected from feed materials permitting liquid/solid conversion, so that a definite shape resembling that of the feed "pellet" may be imparted thereto and set.

Two classes of feed binding agents may be used: - binding agents used in a solvent or dispersant medium, - . agents capable of being melted.

Among binding agents used in a solvent or dispersant medium, there may be mentioned: - the class of hydrocolloids such as, in particular, water-soluble derivatives of cellulose, such as: carboxymethyl- cellulose, hydroxypropylcellulose, hydroxyethylcellulose, hydroxymethylcellulose, - the class of natural or synthetic polysaccharides such as: gum arabic, gum tragacanth, carrageenates, dextrins, starch, xanthan gum, alginates, - sugars, - molasses and vinasses, lignosulphonates, - grain flours or seaweed meal, - the class of crystallizable inorganic compounds such as lime, plaster, sodium silicate, calcium carbonate and silica, - gelatins, - tanned proteins, - polyvalent cation salts of natural or synthetic polyacids, - drying oils and mastics obtained by the combination of a drying oil and a filler.

Some binding agents are used with crosslinking agents selected, for example, from aldehydes for proteins, salts or oxides of di- or trivalent metals for alginates, xanthan gum, molasses, vinasses and other curing agents suited to the binding agents used and well known to those skilled in the art.

Among binding agents capable of being melted, there may be mentioned, by way of examples: - fatty acids and alcohols, - hydrogenated vegetable and animal fats, 8 - glycerol esters, - paraffin waxes, - natural or synthetic waxes, - synthetic polymers such as polyethylene glycols, polyvinyl acetate, etc.

Among all the binding agents, it is preferable to use molasses, vinasses, fatty acids, hydrogenated vegetable or animal fats, plaster and paraffin waxes.

Additives which enable the pellet to be provided with the desired qualities of density, mechanical strength and rapid disintegration in the rumen may be introduced into the special pellet according to the invention.

By way of useful additives for the preparation of the special pellets according to the invention, there may be mentioned: - inorganic additives such as: silica, silicates, talc, clays, calcium carbonates, phosphates. - additives derived from natural products such as: grain flours, residues of the cereals and wood industries, ground feed cakes, various brewery and fermentation residues, cellulose vegetable fibres, polysaccharides and sugars.

The binding agent, supplemented where appropriate with additives, preferably represents 40 to 95 % of the mass of the "special pellet according to the invention" . The content of inorganic or natural additives represents from 0 to 80% by weight relative to the binding agent.

The mixing of the binding agent and the protected product may be carried out at. the same time as the shaping or beforehand. The shaping may be carried out by means of a die or a mould.

The nature of the binding agent, the pouring temperature and the quantity of additives will be adapted by those skilled in the art in accordance with the quality of the desired special pellet according to the invention: - its appetency, - its density, - its shape, - its size, - its mechanical strength, - its solubility, - its ability to disintegrate in the rumen.

They take the form of sticks, preferably cylindrical, possessing, in particular, average sizes of 4 to 20 mm in length and 4 to 10 mm in diameter.

The special pellets according to the invention possess at least three features which make them useful for the feeding of ruminants: 1/ They are miscible in all proportions with the granulated feeds generally distributed to animals as a supplement to the basic feed ration. That is to say, they can withstand without unmixing the different 10 steps of handling to which granulated feeds are subjected, and become integrated in the feed distribution system. 2/ Loss of protection of the protected active principles is limited therein during shaping. 3/ The "special pellets according to the invention" thus produced disintegrate rapidly in the rumen and, on mastication during rumination, avoid a loss of protection of the active principles included. The protected active principles can then continue their passage freely. 4/ The capacity for miscibility with traditional granulated feeds depends essentially on the shape and density of the products produced, and presents no problems for those skilled in the art.

The extent of protection which characterizes the protected principles is equal to 100 minus the extent of release observed in vitro by measurement of the release of the active principles after 24 h in 1,000 ml of pH 6 buffer with stirring at 300 rpm at 40°C. The extent of release represents the percentage proportion of active principles released during the test. The size of the test sample is dependent on the nature of the active principle and its content. For the amino acids mentioned as examples, the test is carried out on approximately 6 g of equivalent.

The extent of protection should naturally be as high as possible. 11 The disintegration of the "special pellets according to the invention" in the rumen, which permits release of the protected active principles, is assessed by incubation in the rumen of fistulated cattle by means of sachets made of nylon fabric with a mesh aperture of 350 microns. The disintegration time should be as short as possible, and especially less than 48 h.

The present invention will be described more completely by means of the examples which follow, which cannot be considered to be limiting in respect of either the protected active principles or the binding agents used.

The protected active principles used for the examples are granules approximately 2 mm in diameter composed of: Type A protected active principle: Particles of lysine monohydrochloride and methionine in the proportion by weight 75:25, containing approximately 12 % of a binding agent consisting of a mixture of stearic acid containing 5 % w/w of 2-vinylpyridine-co-styrene copolymer, protected against degradation in the rumen by a coating layer representing 16 % by weight of the protected product, this layer being composed of a mixture of 30 % of 2-vinylpyridine-co-styrene copolymer, 60 % of talc and 10 % of stearic acid.

The extent of protection of the type A granules is 97 %. „ 12 Type B protected active principlet Particles of lysine monohydrochloride and methionine in the proportion by weight 75:25, containing approximately 12 % of a binding agent consisting of a mixture of stearic acid containing 5 % w/w of 2-vinylpyridine-co-styrene copolymer, protected against degradation in the rumen by a coating layer representing 12 % by weight of the protected product, this layer being composed of a mixture of 20 % of 2-vinylpyridine-co-styrene copolymer and 80 % of stearic acid.

The extent of protection of the type B granules is 99 %.

The type A and B products used for the feeding of ruminants are described in Patents US 4,181,708 and EP 260,186.

EXAMPLE 1 2 % by weight of type A granules are introduced into a mixture of flours intended for the feeding of livestock, and made into the form of a granulated feed in a KAHL rotary die press after steam treatment in accordance with the traditional method of preparation of granulated feeds. The product obtained takes the form of extruded cylinders 5 mm in diameter and approximately 15 mm in length.

The residual extent of protection of the amino acids used for the example is 0 % in, the granulated feed after passage through the jpress. 13 EXAMPLE 2 2 % of type B granules are introduced into a mixture of flours intended for the feeding of livestock/ and made into the form of a granulated feed in a KAHL rotary die press after steam treatment in accordance with the traditional method of preparation of granulated feeds. The product obtained takes the form of extruded cylinders 5 mm in diameter and approximately 15 mm in length.

The residual extent of protection of the amino acids used for the example is 0 % in the granulated feed after passage through the press.

Examples 1 and 2 show that making this type of product into the form of a granulated feed by traditional methods leads to a substantial total degradation of their protection against degradation in the rumen, and consequently to loss of their efficacy for the feeding of ruminants.

EXAMPLE 3 Granules containing active principles protected against degradation in the rumen, and miscible in all proportions with the traditional granulated feed, are obtained in the following manner: Granules of type A protected active principle are introduced into the cavities of a mould. The cavities are frustoconical in shape, 20 mm in height and 8 mm and 10 mm in diameter at the ends.

A molten binding agent is injected under 14 pressure into the porous structure of the particulate bed thus produced in each cavity.

The finished product is recovered by releasing from the mould after solidification of the binding agent on cooling.

The binding agent used for the example possesses the following composition: stearic acid 33.33 % palmitic acid 22.22 % calcium carbonate 22.22 % fermentation residue 22.22 % (reference EUROLYSINE PL 73) The extent of protection and the amino acid titre in the final product are given in Table I.

EXAMPLE 4 Granules containing type A active principles protected against degradation in the rumen, miscible in all proportions with the traditional granulated feed, are obtained by the moulding technique described in Example 3, with the use of a molten binding agent composed of:. stearic acid 30 % palmitic acid 20 % glyceryl monostearate 50 % The extent of protection and the amino acid titre in the final product are given in Table I.

EXAMPLE 5 Granules containing type A active principles 15 protected against degradation in the rumen, miscible in all proportions with the traditional granulated feed, are obtained by the moulding technique described in Example 3, with the use of a molten binding agent composed of: stearic acid 16.67 % palmitic acid 11.11 % glyceryl monostearate 27.78 % calcium carbonate 44.44 % The extent of protection and the amino acid titre in the final product are given in Table I.

EXAMPLE 6 Granules containing type A active principles protected against degradation in the rumen, miscible in all proportions with the traditional granulated feed, are obtained by mixing type A granules with a binding agent composed of: plaster 22.73 % calcium carbonate 45.45 % water 31.82 % The mixture is made into the form of particles measuring approximately 20 mm by 10 mm, by pouring onto a non-adhesive support and recovery after drying in an oven.

The extent of protection and the amino acid titre in the final product are given in Table I.

EXAMPLE 7 Granules containing type A active principles 16 protected against degradation in the rumen, miscible in all proportions with the traditional granulated feed, are obtained by mixing type A granules with a binding agent composed of: plaster 25.32 % microcrystalline cellulose 18.99 % water 55.70 % The mixture is made into the form of particles measuring approximately 20 mm by 10 mm, by pouring onto a non-adhesive support, the particles being recovered after drying in an oven.

EXAMPLE 8 Granules containing type B active principles protected against degradation in the rumen, miscible in all proportions with the traditional granulated feed, are obtained by mixing type B granules with a binding agent composed oft plaster 29.41 % calcium carbonate 58.82 % water 41.18 % The mixture is made into the form of particles measuring approximately 20 mm by 10 mm, by pouring onto a non-adhesive support and recovery after drying in an oven.

The extent of protection and the amino acid titre in the final product are given in Ta£le I. 17 EXAMPLE 9 Granules containing type B active principles protected against degradation in the rumen, miscible in all proportions with the traditional granulated feed, are obtained by mixing type B granules with a binding agent composed of: plaster 25.32 % macrocrystalline cellulose 18.99 % water 55.57 % The mixture is made into the form of particles measuring approximately 20 mm by 10 mm, by pouring onto a non-adhesive support and recovery after drying in an oven.

EXAMPLE 10 Granules containing type A active principles protected against degradation in the rumen, miscible in all proportions with the traditional granulated feed, are obtained by mixing type A granules with a binding agent composed of: beet molasses 76.92 % calcium oxide 23.08 % The mixture is made into the form of particles measuring approximately 20 mm by 10 mm, by pouring onto a non-adhesive support and recovery after spontaneous curing.

The extent of protection and the amino acid titre in the final product are given in Table I. 18 EXAMPLE 11 Granules containing type A active principles protected against degradation in the rumen, miscible in all proportions with the traditional granulated feed, are obtained by mixing type A granules with a binding agent composed of: molasses 71.43 % gelatin 14.29 % water 14.29 % The mixture is made into the form of particles measuring approximately 20 mm by 10 mm, by pouring onto a non-adhesive support and recovery after gelling.

EXAMPLE 12 Granules containing type B active principles protected against degradation in the rumen, miscible in all proportions with the traditional granulated feed, are obtained by mixing type B granules with a binding agent composed of: molasses 71.43 % gelatin 14.29 % water 14.29 % The mixture is made into the form of particles measuring approximately 20 mm by 10 mm, by pouring onto a non-adhesive support and recovery after gelling. 19 The extent of protection and the amino acid titre in the final product are given in Table I.

Table I summarises the extent of protection observed for the protected active principles used in the examples, after making into the form of "special pellets according to the invention".

It also shows that the judicious choice of the composition of the binding agent enables the rate of disintegration of the said granules in the rumen to be adjusted.

It is understood that the method of making into the form of special pellets according to the invention, by agglomeration in the presence of a binding agent, described in the present invention, may be applied to an extremely wide range of active principles protected against degradation in the rumen, by matching the physicocheroical features of the binding agent to the nature of their protection. The pH of the binding agent, the temperature at which it is used and its compatibility or its solvent power with respect to the composition protecting the protected active principle in question should be taken especially into consideration.

TABLE I Characteristics of the products produced: EXAMPLE 13 Granules containing type B active principles protected against degradation in the rumen, miscible in all proportions with the traditional granulated feed, are obtained by mixing type B granules with a binding agent composed of: clay 50 % soya flour 12.5% aqueous 4% CMC solution 37.5% The mixture is made into the form of particles of about 8 mm diameter by extrusion across a die. The canes thus obtained are dried in a ventilated oven and reduced to elements about 20 long.

The level of B in the final agglomerated product was 37.5 % (by weight). The extent of disintegration of the final product in the rumen after 6 hours was 100% (by weight). The extent of protection of the active principle in the final product was 99%.

EXAMPLE 14 Granules containing type B active principles protected against degradation in the rumen, miscible in all proportions with the traditional granulated feed, are obtained by mixing type B granules with a binding agent composed of: dolomite 59.7% soya flour 14.9% aqueous 4% CMC solution 25.4% The mixture is made into the form of particles of about 8 mm diameter by extrusion across a die. The canes thus obtained are dried in a ventilated oven and reduced to elements about 20 long.

The level of B in the final agglomerated product was 37.5 % (by weight). The extent of disintegration of the final product in the rumen after 6 hours was 100% (by weight). The extent of protection of the active principle in the final product was 89%.

* CMC: Carboxymethyl cellulose, sodium salt 96899/2 ;» 22

Claims

1. Compositions in the form of "pellets", as herein defined^ containing granular active principles protected against degradation in the rumen, used for the nutritional and/or medicinal supplementation of ruminants, releasing the said active principles in the abomasum and/or the intestine, characterized in that they are obtained by mixing the protected active principle in granular form and a binding agent selected from binding agents capable of being solubilized, crosslinked or melted, and optionally a disintegrating agent and/or a filler.

2. Compositions according to claim 1, characterized in that the active principle is selected from vitamins, amino acids and drugs protected from degradation in the rumen.

3. Compositions according to claim 2, characterized in that the protected active principle is selected from amino acids, vitamins and drugs protected by a pH-sensitive copolymer, a natural product or an enzymatically degradable product.

4. Compositions according to claim 3, characterized in that the protected active principle is selected from amino acids, vitamins and drugs protected by a pH-sensitive copolymer based on vinylpyridine and on styrene in combination with a hydrophobic substance.

5. Compositions according to claim 3, characterized in that the protected active principle is 23 selected from amino acids, vitamins and drugs protected by a natural product or an enzymatically degradable product selected from zein or chitosan.

6. Compositions according to any one of the preceding claims, characterized in that the protected active principle takes a granular form of average diameter between 0.3 and 5 mm.

7. Compositions according to claim 1, characterized in that the binding agent capable of being crosslinked consists of a hydrocolloid selected from alginates, gelatins, cellulose derivatives, polysaccharides, molasses or vinasses.

8. Compositions according to claim 7, characterized in that the crosslinking agent is selected from aldehydes for proteins, salts or oxides of di- or trivalent metals for alginates, xanthan gum, molasses and vinasses.

9. Compositions according to claim 1, characterized in that the binding agent capable of being melted is selected from fatty acids, fatty alcohols, glycerol esters, polyethylene glycols, paraffin waxes, natural or synthetic waxes and hydrogenated animal or vegetable fats.

10. Compositions according to claim 1, characterized in that the disintegrating agent is selected from grain flours, ground feed cakes, brewery and fermentation residues, cereal and wood by-products and cellulose fibres.