ES2289923B1 - PREPARATION BASED ON VEGETABLE EXTRACTS FOR ANIMAL FEEDING. - Google Patents

Abstract

A product consisting of a plant extract or one or more of its main components, of natural origin or reproduced by synthesis, fixed on a porous inorganic support consisting mainly of precipitated silica, and coated with a protective layer consisting of an emulsifier, of the mono- and / or diglycerides type of fatty acids, or of their derivatives esterified with acetic, lactic acid or the like. A procedure for preparing said product is also described. This type of product has application in animal feed.

Description

Preparation based on plant extracts for animal feeding.

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Area of application

A product constituted based on a vegetable extract absorbed and / or adsorbed on a support inorganic and coated by a protective layer based on an agent non-phonic surfactant. A procedure is also described to make this product.

This type of products has an effect like antibacterial agents and are useful in animal feed contributing to the improvement of the general state of the animal. Some of These products actively promote the growth of flora beneficial and simultaneously inhibit the development of pathogens. Many of them have utility as appetite stimulants and Food flavorings.

In the denomination of plant extract in the This report should be considered including both the extract natural vegetable like the one that is obtained synthetic route. This definition also includes the main components obtained at from the extract or prepared by synthesis.

Description of the problem

The prohibition of a large part of the agents antibacterials that have been used as additives in the animal feed in recent years has caused more interest in the search for alternative products, mainly of Natural origin, to replace these products.

Since ancient times the beneficial action of multitude of plant extracts. An example of great interest is related to the antibacterial activity of oregano oil, caused by its main components, phenols, carvacrol and thymol Similar effects presents the essential oil of anise, and of Its main component, anethole. There are other cases described in the bibliography, such as, the antiseptic activity of peppermint or of the essential oil of eucalyptus, the anti-inflammatory activity of Cinnamon, licorice antidiarrheal, among many others.

While these were traditionally used natural extracts in the treatment of conditions in humans and animals, it has not been until recently that they have recovered a notoriety that they had lost.

In fact, the limiting factors that have been revealed when generalizing its use are related to the following aspects:

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Dosage of natural extracts, that is, quantity of each of the components that constitute the abstract.

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Correct formulation, that is, nature and quantity of adjuvants and excipients for Premix elaboration.

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Adequate protection of the extract itself and its components against degrading processes.

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Bioavailability, i.e. release of the active ingredients at the time and place adequate.

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He intense flavor of these oils, which produces in many cases a rejection for ingestion, especially in young animals, which They are more likely to suffer from conditions.

As set out below, the review The state of the art shows several attempts described and claimed to solve the problems associated with the use of natural extracts in medicine and veterinary medicine.

Most of them, although they can solve one or several of the problems raised, such as those associated with the correct dosage, suffer from other problems, such as adequate protection of the active ingredients, which causes low stability, incorrect release or premature degradation.

In addition, effective solutions have not been proposed. for the problem of rejection of ingestion of oils due to its bad taste This is usually the reason why many animals, especially the youngest, do not ingest natural extracts hindering, therefore, the treatment.

In conclusion it is found that to date there is no global solution to all the problems raised that allow, therefore, the development with guarantees of a treatment effective based on natural extracts.

State of the art

A brief summary of the state of the art in which references have been included most relevant bibliographies.

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One of the first antecedents is European patent EP0835120 of June 1996, in which antimicrobial pharmaceutical compositions constituted based on essential oils obtained from Origanum vulgare are claimed, together with a pharmaceutically acceptable carrier.

This patent claims a% of thymol + carvacrol greater than 55% in the plant extract and a greater than 10: 1 ratio of carvacrol versus thymol.

Likewise, in the said patent claim methods for using said compositions in the treatment of many diseases, such as mastitis, dermatological and ophthalmological conditions, among others.

In the same year, the EP patent was filed 828502, May 1996, in which the compositions are claimed Pharmaceutical and veterinary in which the active substance is among others, the essence oil of oregano in a proportion between 1 and 15%, and in which the excipient can be selected from a great variety, paraffin, starch and its derivatives, carbonate Calcium, among others.

This patent also claims the application of this type of compositions in prevention and treatment of gastro-intestinal disorders of microbial origin

A more recent antecedent is the constituted by EP 1178736 of May 1999, which describes and claims the action of carvacrol and thymol and their mixtures as bactericidal products

There are some examples of Essences or aromas formulations used in industry cosmetic and also in food. An example is described in Perfurmer and Flavorist, 52-55, vol. 27, (2002). In this article some considerations are made about a encapsulation procedure in order to protect the aroma throughout the subsequent elaboration of the cosmetic or the food.

Descriptive memory

A product is described herein. in which all the problems associated with the use of plant extracts useful in food animal, guaranteeing the following aspects:

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Correct extract dosage plant by fixing a defined concentration on a support inorganic.

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Adequate formulation for being the active ingredients adsorbed and / or properly absorbed due to the special characteristics of the support.

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Protection against degradation by the action of a protective film that covers the principles assets.

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Stability due to the solid fixation of the protective agent, an emulsifier, to the support.

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Release at the time and place suitable, within the organism of the animal, due precisely to The nature of the protective agent.

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Elimination of the effect produced by the intense flavor, due to the presence of the layer protective

As a result of all this you get a maximum efficiency by taking advantage of the antibacterial effect of the active ingredients used

In essence, the invention consists in fixing of a plant extract or its components in a support inorganic porous, consisting mainly of silica precipitate, and the subsequent coating with a protective layer, constituted by an emulsifier, of the mono and / or diglyceride type of saturated fatty acids, or their derivatives esterified with acetic, lactic acid or similar.

It is also within the scope of this invention the procedure for carrying out the preparation of the product. A detailed description of the more relevant technical aspects, as well as, of some examples that They illustrate such preparation.

Finally, within the scope of this invention should be considered the application of the product as well elaborated in nutrition and veterinary medicine.

The usefulness of these products lies in the fact that they promote flora growth very effectively intestinal beneficial and simultaneously inhibit growth of pathogens.

The most positive effect is manifested in the periods of imbalance in young animals, when they suffer important changes in their diet, such is the case, of weaning. At this time, there are significant deteriorations in its intestinal flora, in whose regeneration, the products subject to The present invention has shown a very positive effect.

In general, it can be used in all types of animals, mainly, in young people. Thus, it shows effects beneficial in pigs, calves, cattle in general, rabbits, birds, and even, they are useful in pets.

Advantages as described

Against what is described in the bibliography, the product described here represents important advantages that They are collected below.

As indicated above there are some plant extracts whose antimicrobial activity is known since ancient times. When in this memory the active ingredients, refers to plant extract, as well as main components of natural origin or reproduced by synthesis.

One of the most important sections in the development of the present invention is related to the support Inorganic used. The bibliography collects some examples of "carriers" or brackets used for fixing a oily liquid on a solid. It is usual to find references envelope, carbonates, such as calcium or sodium, sulfates, such as, sodium, magnesium or calcium, and even polymers, along with some others.

In most of the examples described in the bibliography, the liquid product is not good enough fixed to the support producing separations, which originates, in many cases, concentration gradients, heterogeneities and, by therefore, important problems of correct dosage.

In order to solve this problem, raised the use of a support based on silica precipitated, which represents an important advance and an improvement in front of everything described.

The precipitated silica used is constituted by spherical particles of a size between 80 and 500 microns. Be deals with regular microporous particles whose features are optimal to achieve the goal of setting the active substance and transport it effectively.

A size and shape of particles such as used have a number of advantages. On the one hand, it is avoided the formation of dust that would accompany smaller sizes. For other, and if compared with particles of larger size, the specific surface and therefore the fixing capacity of extract per unit of weight.

Moreover, the fact that it is about microporous structure represents an important advance, in the sense that the specific surface area increases considerably allowing both mechanisms, adsorption and absorption, necessary to set significant amounts of principle active.

As advanced previously, once deposited the active substance in the inorganic support, it is submitted to a coating with a protective layer.

The nature and characteristics of bliss protective layer have very important advantages over all described earlier in the bibliography.

First, as has been advanced, the protective layer is made by coating using mono and fatty acid diglycerides, referred to within the code E-471 food. Optionally, they can be used its esters included in the code E-472. These products are included as feed additives, within the group of stabilizing and emulsifying products.

This product is a non-surface active agent. phonic, which represents an important novelty against used in the literature In fact this feature is a consequence of the presence in its molecule of a lipophilic part and other hydrophilic This strong molecular polarity favors its fixation to inorganic support.

In addition, the tensile nature of the Coating represents many other advantages. Are especially important those related to the significant increase in protective capacity over the active substance, especially if compare with the examples in the bibliography where you don't know contemplates no coating mechanism.

On the other hand, nature lipophilic-hydrophilic of this coating results from very useful in regard to its bioavailability. So, when the animal ingests this product, correctly formulated, the Lipophilic layer prevents the release of the active substance. So, when the product has reached its target, within the body of the animal, there is a controlled release effect and therefore a significant increase in activity is achieved.

Clearly, if you can control the release of the active substance in the gastrointestinal tract, the problem of the intense flavor associated with the Most essential oils. This section has a great importance given that the animal that is subjected to this treatment He is usually young and, therefore, reluctant to ingest products of Taste not very nice.

In certain cases it can be important favor a more controlled release of the active substance. In In these cases it is advisable to reduce the surfactant nature of the covering. In these cases, this decrease can be achieved lowering the polarity of the hydrophilic part of the emulsifier used in the coating by esterification of the OH free of glycerin in the mono- and diglycerides that constitute the E-471

The esterification can be carried out with formation of acetic, lactic and similar esters of mono and diglycerides This type of compounds is described with the code E-472 and included in the same group of emulsifiers of legislation on food additives.

In this way, one or the other can be used type of coating, depending on the needs of the treatment, which represents an obvious advance regarding previously described.

Detailed Description of the Invention

The object of the present invention is to a product consisting of a plant extract, or, of its main components of natural origin or reproduced by synthesis, fixed, by adsorption and / or absorption on a support inorganic porous consisting mainly of silica precipitated, and coated with a protective layer consisting of an emulsifier, of the mono- and / or diglyceride type of fatty acids saturated, or, of its acid esterified derivatives acetic, lactic or similar.

They are also part of the purpose of this invention the process of preparing said product, whose detailed description is made later and that in essence are based on the use of a fluid bed or a mixer for fixing and coating of the active substance.

Within the object of the present invention also include applications in nutrition and medicine veterinary As noted above, some of These products have the ability to promote the growth of beneficial flora simultaneously inhibiting pathogens, especially in young animals. In this way they reestablish the disturbed equilibrium in periods in which changes occur in the feeding of these.

As progress has been made, in the elaboration of product are considered three fundamental sections: the extract Vegetable, inorganic support and protective layer.

As for the plant extract it is a natural extract obtained from vegetables by the methods usual such as steam distillation, extraction with solvents, expression; Composition products are obtained variable such as essential oils, resins, oleoresins or mixtures of them.

In the scope of this invention also consider plant extracts natural extracts reproduced by synthesis, as well as its main components of natural origin or obtained via synthetic.

Among the most common natural extracts, mention is made of the essential oil of oregano from plants of the genus Origanum and Thymus , and whose antimicrobial activity has been known since ancient times. It is also reported that its active ingredients Timol and Carvacrol, promote the increase of gram-positive lactic bacteria in the intestine and the reduction of pathogenic bacteria (Varel, VH 2001 Varel, VH 2001, Current Microbiology 44: 38-43). A similar effect has been described in aniseed oil, a product from plants of the genus Pimpinella , and its components, mainly anethole. In addition to this property, many applications of aniseed oil have been reported in animal feed, and even human, related to the treatment of conditions
gastric

There are other examples such as garlic essential oil with high antiparasitic and antiseptic activity, cinnamon essential oil useful in inhibiting the development of the fungus Aspergillus flavus . These are a few examples within a long list of plant extracts for animal feed.

The active substance is deposited on a support inorganic consisting basically of precipitated silica.

On the one hand, the support is completely inert, in the sense that it does not react with the active substance and, therefore, does not cause or induce any kind of process of degradation.

Moreover, the characteristics physicochemical of this support are perfectly appropriate to the intended utility. It's about particles spherical with an approximate size of between 80 microns to about 500 microns

The precipitated silica has a very suitable characteristic for the formulation of liquids. Be It's about your microporosity. The particles contain a multitude of pores that logically increase the specific surface area with respect to  similar particle sizes of other types of supports. But, in addition, the active substance penetrates into said pores and is occluded in them. The result is evident, increases the load capacity and In addition, it guarantees its fixation in the support.

Different methods can be used to fix The active substance in the support. The most appropriate procedure It involves the use of a fluid bed. It's about keeping the silica suspension in a bed and spray the plant extract in form of small micro-drops that are put in very intimate contact with the particles of the support. In this way the adsorption and absorption processes achieving a correct fixation.

An alternative to the procedure described It consists of the use of mixers. Within this type, the that fluidize the load are the most convenient, such is the case of a Forberg mixer. In them, the mixing times are even less than 5 minutes.

In all cases, the support would remain in continued movement and on it the spray would be sprayed or fogged vegetable extract Mixing would be maintained, while stirring. adequate temperature until oil level is reached on the stand Acceptable results are achieved with times of stirring for 30 minutes to 3 hours, at temperatures between 15 ° C and 40 ° C,  depending on the characteristics of the mixer used.

In both procedures you can add the plant extract or its components previously dissolved in a suitable solvent. Examples of these solvents are hexane, methanol, ethanol and the like. In this case, when the Dosing and mixing process, the product is subjected to a complete deolventization process using the methods common, such as vacuum evaporation, dried in the bed fluid, or some other.

With either procedure, reach concentration values that are considered adequate for this type of products, that is, on the order of 20% to 30% or higher.

The third phase in product development object of the present invention consists in coating the plant extract deposited on the precipitated silica with a protective layer.

For this phase an agent has been selected emulsifier commonly used as a food additive. Be treats mono- and diglycerides of saturated fatty acids, additive to which corresponds the code E-471.

This emulsifying agent is added directly to the fluid bed or to the mixer, where the extract is located vegetable fixed on the support, producing a dispersion homogeneous on the surface of the support and, therefore, giving rise to a very effective protective layer.

It is important to note that, as it has been cited above, the active substance is dosed reaching concentrations that are in the order of 30%. One of the reasons of not excessively increasing this proportion of principle active, resides in that, active centers must be left in the support inorganic to subsequently fix the protective layer.

It has been possible to evaluate what concentrations of 10-20% order of mono- and diglycerides are enough to carry out an effective coating. They are usual values of the order of 10% to 14% emulsifier.

As for its physical characteristics, it is important to note that fatty acid esters are used with the so that they are solid at room temperature and, with points of melting above 70 ° C. This parameter is very important as as the solid coating of the active ingredient in the support makes degradation agents less permeable than if it were liquid.

The good stability results, dosage at the right time or point and its correct release, therefore, its bioavailability, are factors related to the surface activity of the coating. Is important to note that the additive E-471, for being a non-phonic surfactant exhibits excellent behavior in as for its hydrophilic fixation and its lipophilic resistance.

Table I collects a series of data. obtained throughout the studies carried out since 2003 in a product based on oregano oil. In these trials you controlled the evolution of the concentration of the components main thymol and carvacrol in the feed.

TABLE I Residual activity of thymol and carvacrol in the feed during storage, after heat treatment to 85 ° C

one

The results collected in this table show manifest the high product stability. This effect is justified by the presence of the protective layer.

In some cases it is interesting to decrease the polar character of the coating, for example, when need a slower release in a hydrophilic medium. In these cases you can replace the coating based on mono and fatty acid diglycerides, by their corresponding derivative esterified For the elaboration of this last product, they use short chain organic acids, such as acetic, lactic and similar. In this way the additives are prepared authorized in food and included in the code E-472

The correct dosage of the protective agent is get sprayed in the fluid bed or in the mixer used in the previous phases. Depending on the type of equipment selected and the conditions used, the emulsifying agent it can be dosed in several ways such as molten or in aqueous dispersion

The elaboration of the product ends with a eventual drying, with elimination, if present, of most of the water in the environment, until reaching values of the order 5% or less.

Throughout 2003 and later it has tested the product claimed in the present invention. The results obtained show high efficiency and good Product behavior when used in food animal.

A series of examples are collected below. that show ways of carrying out the invention but not They are limited in any way.

Example one

In a 5 liter capacity flask, it introduce:

1500 g of carvacrol / thymol vegetable extract,

and mix with:

321 g of hexane

This solution is absorbed on:

1100 g of sipernat 2200.

This proportion corresponds to the maximum power of absorption of sipernat. In this way all the particles of sipernat are loaded with oil solution more or less fixed essence / hexane.

Hexane is then evaporated by subjecting the mixture excited under vacuum at a temperature of 30 ° C.

Once the solvent is removed, each particle It contains a portion of vegetable extract and maintains a capacity remnant to absorb more liquid.

Subsequently 390 g of a mixture of mono and diglycerides of molten stearic acid, which it is deposited on the surface of the extract particles vegetable-sipernat.

Example 2

500 kg of vegetable extract are prepared carvacrol / thymol that are absorbed in 370 kg of sipernat 2200.

To carry out this process you must ensure two conditions, which define the set of equipment industrial to be used:

\ ding {226} On the one hand, that the sipernat is is in a state of fluidization. This state can be achieve by means of a fluid bed driven by air flow or in a Forberg shovel mixer.

\ ding {226} On the other, that the droplet size of the plant extract is substantially less than the size of Sipernat 2200 particle, that is, sizes smaller than 100 They would be desirable.

Once the plant extract is fixed, the mixture of mono and diglycerides at a temperature at which this product is in a liquid state, that is, at a temperature above 70 ° C.

The product thus obtained is suitable for post processing

Example 3

For a fixed amount of the amount of if you can change the relative proportions of extract vegetable and coating, taking into account what next:

\ ding {226} As the content in plant extract and increases that of the protective agent, the quality of the coating increases but so does the price / activity ratio as wealth decreases in principle active.

\ ding {226} As the content increases in plant extract and the protective agent decreases, the coating quality but decreases the ratio price / activity as wealth increases in active substance.

Therefore, at the practical level any Active ingredient dosage, protective agent and support inorganic should be done considering the application and costs required

Claims (18)

1. A product consisting of an extract vegetable or one or more of its main components, of natural origin or reproduced by synthesis, fixed on a support inorganic porous consisting mainly of silica precipitated, and coated with a protective layer consisting of a emulsifier, of the mono- and / or diglyceride type of fatty acids, or either, of its derivatives esterified with acetic, lactic acid or Similary. 2. A product according to claim 1 wherein the vegetable extract is the essential oil of oregano, a natural product extracted from the plants of the genus Origanum and Thymus . 3. A product according to claim 1 in the that the plant extract consists of a mixture of Carvacrol and Timol, both of natural origin, and obtained by chemical synthesis 4. A product according to claim 1 wherein the plant extract is the essential oil of anise, a natural product extracted from the plants of the genus Pimpinella , as well as its main components, natural or reproduced by synthesis. 5. A product according to claim 1 wherein the vegetable extract is the essential oil of garlic, a natural product extracted from the Allium plants. 6. A product according to claim 1 wherein the vegetable extract is cinnamon essential oil, a natural product extracted from the Cinnamomum plants. 7. A product according to claims 1 to 6 in which the inorganic support is precipitated silica with a particle size between 80 and 500 microns, preferably between 90 and 300 microns. 8. A product according to claims 1 to 7 in which the coating consists of a mixture of mono and saturated fatty acid diglycerides, preferably acid stearic 9. A product according to claims 1 to 7 in which the coating consists of a mixture of mono and saturated fatty acid diglycerides, preferably acid palmitic 10. A product according to claims 1 to 7 in which the coating consists of a mixture of mono and saturated fatty acid diglycerides in which the group Residual hydroxyl is esterified with acetic acid. 11. A procedure for the elaboration of product according to claim 1 consisting of fixing a plant extract or one or more of its components on a inorganic support based on precipitated silica and its subsequent coating with a layer of protective agent of the mono type and / or diglycerides of fatty acids or their esters. 12. A method according to claim 11 in which the plant extract is deposited on the support inorganic as a solution in an organic solvent volatile, and in which, before coating the product, the solvent 13. A method according to the claims 11 and 12 in which the fixation of the plant extract is carried out on a fluid bed of the inorganic support. 14. A method according to the claims 11 and 12 in which the fixation of the plant extract on the support inorganic is carried out inside a shovel mixer, which guarantees an effective mix. 15. A method according to the claims 11 to 14 in which the protective agent is deposited at a temperature above 70 ° C, preferably between 75 ° C and 85 ° C. 16. The use of the product according to the claim 1 in animal feed and veterinary medicine. 17. The use of the product according to claims 2 and 3 to promote the growth of the flora intestinal beneficial and inhibit the development of pathogens in young animals, preferably in periods of imbalance caused by changes in food. 18. The use of the product according to claims 16 and 17 for the improvement of the general condition in the animals, preferably in calves, birds, pigs, rabbits and companion animals