WO2021234168A1 - Pigment composition and uses thereof - Google Patents

Abstract

The invention relates to a pigment composition comprising at least one xanthophyll pigment, and a matrix, the pigment being dispersed in said matrix, said matrix being a crystalline matrix consisting essentially of hydrogenated fatty acids and of at least one support.

Description

Pigment composition and its uses

The invention relates to a pigment composition, and its uses in the food industry.

From a consumer point of view, the color of food products play a very important role in their attractiveness and palatability.

In particular, the coloring of the yolk of the egg or the color of the meat are qualitative criteria that play an important role in their sensory perception. Indeed, the yellow color of poultry meat is associated with many positive terms by the majority of consumers, while the white color is more associated with terms with negative connotations.

The studies carried out show that this pigmentation is dependent on many factors intrinsic to animals and external, which are in particular of food origin. Indeed, studies have shown the inability of animals to synthesize carotenoids de novo and, consequently, they have highlighted the interest of incorporating these molecules in the ration of animals which are able to assimilate and store pigments from food.

Regarding birds and poultry in particular, the prior art indicates that this yellow pigmentation of flesh and eggs is linked to carotenoid pigments.

Carotenoids are molecules derived from the isoprenoid metabolic pathway and mainly used for their antioxidant and pigmentation properties. Among the carotenoids that pigment, there are xanthophylls (hydrocarbon and oxygen form) as well as certain Apo carotenoids.

Also, the food industry has started to use pigments to increase pigmentation, especially in poultry meat and eggs.

Carotenoid pigments are obtained either by petrochemical synthesis or biologically by producing organisms (algae, crustaceans, plants). The main plant sources of carotenoids in animal feed are corn, corn gluten, alfalfa, alfalfa concentrates and extracts of flowers or plants (paprika). However, the carotenoid content of plant raw materials varies greatly depending on the genetics of the plant, its maturity at harvest, duration and storage conditions.

To cope with the high variability of the carotenoid content in plants (depending in particular on the climatic conditions preceding the harvest) and their coloring efficiency (depending on their chemical structure and their storage stability), synthetic carotenoids are used. introduced into animal feed.

However, the chemical synthesis of these molecules remains expensive, the products derived from them have a weaker antioxidant effect than products of natural origin, and the consumer is less and less inclined to use this type of product, favoring products of natural origin, namely natural pigments.

Also, the use of natural pigments is encouraged.

However, while a protein coat protects the pigment molecule resulting from chemical synthesis and thus prevents its degradation, natural pigments are generally less stable over time regardless of the environmental or storage conditions. Natural pigments are less suitable for industrial applications, especially their inclusion in animal feed.

The aim of the invention is to remedy the stability problems of natural pigments with a view to using them for animal feed.

One of the aims of the invention is therefore to provide a natural composition comprising a stable pigment which does not involve chemical synthesis.

Another object of the invention is to provide a method of manufacturing such a composition.

Also, the invention relates to a pigmenting composition comprising at least one xanthophyll pigment, and a matrix, said at least one xanthophyll pigment being dispersed in said matrix, said matrix being a crystalline matrix essentially consisting of hydrogenated fatty acids, in particular hydrogenated oil, and at least one support.

The invention is based on the surprising finding made by the inventors that a natural pigment, in particular a pigment extracted from plants, can be stabilized, that is to say that, under conventional storage conditions or if it is incorporated in animal feed, its degradation is delayed over time, when it is dispersed within a crystalline matrix as defined in the invention.

By pigmenting composition is meant in the invention a composition which comprises at least one pigment, this pigment being advantageously a natural pigment, that is to say a pigment which does not result from any chemical synthesis, but which results from an extraction from plants.

Xanthophyll pigments are yellow molecules derived from carotenes, by adding oxygen atoms (alcohol, ketone, epoxy functions, etc.), which belong to the carotenoid family. In nature, these pigments are found in plant cells, especially in the petals of certain flowers that are yellow, orange or red.

Throughout the preceding and following description, the terms “at least one xanthophyll pigment” can be uniformly replaced by the terms “one or more xanthophyll pigments” or “a mixture of one type or a mixture of several different types of pigments. xanthophylls'.

In the composition according to the invention, said at least one pigment may be in pure form, or in the form of a plant extract which may be an oleoresin, or else an oleoresin paste obtained from a plant. Said at least one pigment can also be supported by a support for the pigment. We will then speak of supported pigment or pigment on a support. This support for the pigment can be either natural of plant origin, in particular a support of the fibrous residue type of the plant, in particular bagasses, from which the said extract has been extracted, or natural of mineral origin (silica, bentonite, clays of generally, etc ... with the exception of calcium carbonate). In the invention, when reference is made to at least one non-pure pigment, it will be possible to speak of at least one product comprising at least one xanthophyll pigment.

In the invention, said at least one pigment is dispersed, in particular homogeneously, in a crystalline matrix essentially consisting of one or more fatty acids and at least one support.

By "a crystalline matrix consisting essentially of hydrogenated fatty acids and at least one support" is meant in the invention a matrix consisting as essential substances of hydrogenated fatty acids and at least one support. The matrix may further contain other components aimed at stabilizing it, etc., but not participating in the formation of the general architecture of the crystal matrix.

In the invention, by fatty acids is meant carboxylic acids with an aliphatic chain of 4 to 36 atoms. Fatty acids are part of the lipid family. Also in the invention, the terms lipids or fatty acids can be used uniformly for the same meaning.

The composition according to the invention comprises fatty acids, or lipids. This means that it includes several fatty acids of the same nature, or a mixture of several fatty acids of different nature (and therefore of different chemical structures). Therefore, throughout the above and following description, the terms "of fatty acids" may be uniformly replaced by the terms "one or more fatty acids" or "a mixture of one type or a mixture of several different types of fatty acids". 'Fatty acids ".

In the composition according to the invention, the fatty acids are hydrogenated, in particular hydrogenated oil. The hydrogenated fatty acids can be in free form or in the form of monoglycerol, di or polyglycerol fatty acid esters. Also, in the context of a crystalline matrix of the invention composed of fatty acids, this matrix therefore essentially consists of one or more hydrogenated fatty acids, in particular hydrogenated oil, said hydrogenated fatty acids possibly being in the form free or in the form of monoglycerol, di or polyglycerol fatty acid esters.

In another advantageous aspect, the lipids constituting said crystalline matrix are the fatty acids of an oil, in particular a vegetable or animal oil. By way of example and without limiting the scope of the invention, the oils envisaged are in particular the following:

• vegetable oils such as rapeseed oil, oleic rapeseed oil, sunflower oil, oleic sunflower oil, coconut oil, palm oil, palm kernel oil, olive oil, peanut oil, soybean oil, corn oil, mustard oil, castor oil, palm olein, palm stearin, oil safflower, sesame oil, linseed oil, walnut oil, grape seed oil, hemp oil,
• animal oils and fats such as fish oils, in particular oily fish,
• microbial oils derived from so-called oleaginous microorganisms, that is to say capable of storing fatty acids at more than 20% of their dry weight, derived from yeasts, bacteria, in particular of the genus Streptomycès , or microalgae,

or a by-product resulting from the extraction of the aforementioned oils comprising a mixture of fatty acids, such as esterification water, tank bottoms, deodorization condensate, washing water or neutralization pastes.

In the invention, the fatty acids, or the mixture of fatty acids of different nature, are chosen so that the compositions which comprise them are solid, semi-solid or plastic at room temperature, that is to say at room temperature. a temperature between 15 ° C and 40 ° C, in particular from 17 ° C to 30 ° C. These hydrogenated fatty acids are obtained by hydrogenation, in particular catalytic hydrogenation.

In the context of hydrogenation, the triglycerides of an oil are treated for example in the presence of molecular hydrogen and of a catalyst (in particular copper or nickel or palladium) at a temperature of 140 ° C to 250 ° C. . This type of reaction is heterogeneous because there are three phases involved: a gas phase with hydrogen, a liquid phase with the triglycerides to be hydrogenated and a solid phase with the finely divided catalyst. The reaction is exothermic and releases on the order of 100 to 150 kJ per mole of double bond. The hydrogenation can be selective, for example it will be a question of specifically reducing the level of linolenic acid (C18: 3) in an oil to obtain linoleic acid (C18: 2). This type of hydrogenation aims to saturate in a high proportion, or sometimes even completely, the double bonds of the unsaturated fatty acids contained in the triglycerides of an oil.

The hydrogenated oils according to the invention are as follows: refined and hydrogenated palm oil, the melting point of which varies from 60 to 63 ° C, hydrogenated sunflower oil, the melting point of which varies from 69 to 73 ° C. , refined and hydrogenated rapeseed oil with a melting point ranging from 68 to 74 ° C and palm stearin (comprising C16-C18 fatty acids) with a melting point ranging from 56 to 62 ° C.

Other interesting oils in the context of the invention can be used: soybean oil (non-GMO), the melting point of which varies from 68 to 71 ° C or also rapeseed oil (high erucic), comprising saturated fatty acids from C12 or C14, and whose melting point varies from 61 to 66 ° C.

Other oils with melting points, when hydrogenated, greater than or equal to 35 ° C can also be used.

In certain aspects of the composition according to the invention, it is also possible to mix lipids according to the invention exhibiting a high melting point, above 35 ° C., with lipids according to the invention, the melting point of which is below 35 ° C. In this case, it should be ensured that the melting point of the mixture will be above 35 ° C.

For example, it will be possible to produce a mixture of hydrogenated coconut oil, the melting point of which is between 30 and 32 ° C, with one or more hydrogenated oils having a melting point greater than 65 ° C, so that the overall melting point of the mixture of hydrogenated coconut oil and other oils is greater than 35 ° C.

The crystallization temperatures of these same hydrogenated oils are as follows:

around 47 ° C for refined and hydrogenated palm oil,

around 49 ° C for hydrogenated sunflower oil,

around 49 ° for refined and hydrogenated rapeseed oil,

around 37 ° C for palm stearin,

around 48 ° C for soybean oil (non-GMO), and

about 55 ° C for rapeseed oil (high erucic).

The crystalline matrix according to the invention, in addition to the hydrogenated fatty acids, contains one or more supports (of the same or different nature). These supports have the effect of stabilizing and solidifying the composition and in particular of making it possible to solidify the crystalline matrix of hydrogenated fatty acids.

Said at least one support is chosen from silica, calcium carbonate, pyrogenic silica, calcium stearate, magnesium stearate, calcium sulfate, calcium formate, bentonite, calcium phosphate, dextrose, diatomaceous earth or co-products from the first plant processing industry such as tagetes bagasses (fibrous residues of tagetes flower after extraction of pigments), corn cob, remoulding of wheat, seedling of wheat, etc…, or a mixture of these.

The composition according to the invention is characterized by said at least one xanthophyll pigment which is dispersed, in particular homogeneously, in a crystalline matrix essentially consisting of fatty acids and a support, that is to say dispersed in a crystalline matrix essentially consisting of one or more fatty acids and one or more supports.

Said at least one xanthophyll pigment is dispersed in the matrix, so that the pigment is evenly distributed from the surface of the matrix to the core thereof.

Advantageously, we will speak of a homogeneous dispersion so that, macroscopically, the pigment is present throughout the matrix from its surface to the core thereof, so that on average a pigment or a mixture of different types of pigments is equidistant from another pigment or from another mixture of different types of pigments. In addition, this dispersion is such that it is guaranteed that a minimum concentration of pigments can be measured by random sampling in the finished product.

The matrix is said to be crystalline, which means that it forms crystals of fatty acids. These crystals are organized so as to create a network within which said at least one pigment is dispersed.

Advantageously, the invention relates to the aforementioned pigmenting composition, comprising by mass relative to the total mass of the composition:

- from 0.2 to 20% of at least one xanthophyll pigment,

- from 30 to 50% hydrogenated fatty acids, and

- from 10 to 35% of at least one support.

The composition according to the invention therefore advantageously comprises from 0.2 to 20% of at least one xanthophyll pigment and from 40 to 85% of crystalline matrix, the percentages being expressed by mass relative to the total mass of the composition.

Also, in the composition of the invention, said at least one xanthophyll pigment represents by mass relative to the total mass of the composition: 0.2%, 0.3%, 0.4%, 0.5%, 0 , 6%, 0.7%, 0.8%, 0.9%, 1%, 1.1%, 1.2%, 1.3%, 1.4%, 1.5%, 1.6 %, 1.7%, 1.8%, 1.9%, 2%, 2.1%, 2.2%, 2.3%, 2.4%, 2.5%, 2.6%, 2.7%, 2.8%, 2.9%, 3%, 3.1%, 3.2%, 3.3%, 3.4%, 3.5%, 3.6%, 3, 7%, 3.8%, 3.9%, 4%, 4.1%, 4.2%, 4.3%, 4.4%, 4.5%, 4.6%, 4.7% , 4.8%, 4.9%, 5%, 5.1%, 5.2%, 5.3%, 5.4%, 5.5%, 5.6%, 5.7%, 5 , 8%, 5.9%, 6%, 6.1%, 6.2%, 6.3%, 6.4%, 6.5%, 6.6%, 6.7%, 6.8 %, 6.9%, 7%, 7.1%, 7.2%, 7.3%, 7.4%, 7.5%, 7.6%, 7.7%, 7.8%, 7.9%, 8%, 8.1%, 8.2%, 8.3%, 8.4%, 8.5%, 8.6%, 8.7%, 8.8%, 8, 9%, 9%, 9.1%, 9.2%, 9.3%, 9.4%, 9.5%, 9.6%, 9.7%, 9.8%, 9.9% , 10%, 10.1%, 10.2%, 10.3%, 10.4%, 10.5%, 10.6%, 10.7%, 10.8%, 10.9%, 11 %, 11.1%, 11.2%, 11.3%, 11.4%, 11.5%, 11.6%, 11.7%, 11.8%, 11.9%, 12%, 12.1%, 12.2%, 12 , 3%, 12.4%, 12.5%, 12.6%, 12.7%, 12.8%, 12.9%, 13%, 13.1%, 13.2%, 13.3 %, 13.4%, 13.5%, 13.6%, 13.7%, 13.8%, 13.9%, 14%, 14.1%, 14.2%, 14.3%, 14.4%, 14.5%, 14.6%, 14.7%, 14.8%, 14.9%, 15%, 15.1%, 15.2%, 15.3%, 15, 4%, 15.5%, 15.6%, 15.7%, 15.8%, 15.9%, 16%, 16.1%, 16.2%, 16.3%, 16.4% , 16.5%, 16.6%, 16.7%, 16.8%, 16.9%, 17%, 17.1%, 17.2%, 17.3%, 17.4%, 17 , 5%, 17.6%, 17.7%, 17.8%, 17.9%, 18%, 18.1%, 18.2%, 18.3%, 18.4%, 18.5 %, 18.6%, 18.7%, 18.8%, 18.9%, 19%, 19.1%, 19.2%, 19.3%, 19.4%, 19.5%, 19.6%, 19.7%, 19.8%, 19.9% or 20%,

the hydrogenated fatty acids represent by mass relative to the total mass of the composition 30%, 31%, 32%, 33%, 34%, 35%, 36%, 37%, 38%, 39%, 40%, 41 %, 42%, 43%, 44%, 45%, 46%, 47%, 48%, 49% or 50%, and

said support, or said at least one support, represents by mass relative to the total mass of the composition 10%, 11%, 12%, 13%, 14%, 15%, 16%, 17%, 18%, 19 %, 20%, 21%, 22%, 23%, 24%, 25%, 26%, 27%, 28%, 29%, 30%, 31%, 32%, 33%, 34% or 35%.

In view of the aforementioned proportions, a person skilled in the art understands that if he wishes to provide a composition according to the invention comprising by mass relative to the total mass of the composition 50% of fatty acids and 35% of support, he must then limit its amount of pigment to a maximum of 15%. If, on the other hand, he wishes to have a composition in which the fatty acids represent by mass relative to the total mass of the composition 50% and the pigment 20%, he will then have to reduce the amount of support to a maximum of 30%.

In the case where the composition according to the invention is made from a pigment which is not in the pure state, the composition advantageously comprises:

- from 20 to 60% by mass relative to the total mass of the composition of a product comprising at least one xanthophyll pigment, said at least one xanthophyll pigment representing from 1 to 30% by mass relative to the mass of said product comprising at least one xanthophyll pigment,

- from 30 to 50% by mass relative to the total mass of the composition of hydrogenated fatty acids, and

- from 10 to 35% by mass relative to the total mass of the composition of at least one support.

In this case, the pigment which is represented in an amount of 1 to 30% is expressed by mass relative to the mass of the product and not of the total composition. If we now reduce the proportion of pigment to the total mass of the composition, the pigment is therefore present in an amount of 0.2 to 18% by mass.

In the invention, by "a product comprising at least one xanthophyll pigment", it is obviously understood that several products each comprising at least one xanthophyll pigment may be present. If several products each comprising at least one xanthophyll pigment are present in the aforementioned composition, all of these products will represent from 20 to 60% by mass relative to the total mass of the composition, and the total of the pigments contained in said several products will represent from 1 to 30% by mass relative to the total mass of said products.

It is obviously understood in the invention that the product comprising at least one xanthophyll pigment is present by mass relative to the total mass of the composition in the amount of 20%, 21%, 22%, 23%, 24%, 25% , 26%, 27%, 28%, 29%, 30%, 31%, 32%, 33%, 34%, 35%, 36%, 37%, 38%, 39%, 40%, 41%, 42 %, 43%, 44%, 45%, 46%, 47%, 48%, 49%, 50%, 51%, 52%, 53%, 54%, 55%, 56%, 57%, 58%, 59% or 60%, and that the pigment in this product is present by mass relative to the total mass of the product at the level of 1%, 2%, 3%, 4%, 5%, 6%, 7%, 8 %, 9%, 10%, 11%, 12%, 13%, 14%, 15%, 16%, 17%, 18%, 19%, 20%, 21%, 22%, 23%, 24%, 25%, 26%, 27%, 28%, 29% or 30%.

Advantageously, the invention relates to the aforementioned composition, where said at least one xanthophyll pigment is at least one of the following pigments: lutein (of formula C ₄₀ H ₅₆ O ₂ ), zeaxanthin (of formula C ₄₀ H ₅₆ O ₂ ), beta-carotene (of formula C ₄₀ H ₅₆ ) and capsanthin (of formula C ₄₀ H ₅₆ O ₃ ).

Lutein has the following formula:

Zeaxanthin has the following formula:

Beta-carotene has the following formula:

Capsanthin has the following formula:

The pigments are advantageously in their trans form which is the bioavailable form.

In general, in plant extracts comprising xanthophyll pigments, lutein is present in an amount greater than 50% by mass relative to the total mass of pigments; the proportions of the other types of pigments vary.

For example, in the case of a tagete oleoresin, the trans-lutein may represent 80% and more by mass relative to the total mass of pigments, the trans-zeaxanthin, 4.5% and more, the rest of the total mass of pigments being distributed between capsanthin and beta-carotene with varying percentages.

Even more advantageously, the invention relates to the aforementioned composition, where said at least one pigment is obtained from a plant extract, in particular from an extract of marigold.

The composition according to the invention therefore comprises at least one pigment derived from a plant extract. In the invention is meant by plant, all photosynthetic organisms whose cells have a wall made of cellulose. This group is made up of two lineages, the first composed of algae, and the second composed of terrestrial plants including bryophytes (mosses and liverworts), ferns (pteridophytes), gymnosperms and angiosperms.

Pigments derived from extracts of algae and plants are therefore included as well as extracts of algae and plants themselves. These extracts from algae and plants can be obtained from the organism as a whole or, where appropriate, from one of its constituent parts, namely, without being limiting, the fruits, leaves, fibers, the stems, seeds, flowers, bark or even the roots of this organism.

Advantageously, said at least one pigment is obtained from an extract of flowers.

Even more advantageously, said at least one pigment is obtained from an extract of tagetes. Marigolds or tagettes, scientific name Tagetes , are a genus of herbaceous plants of the Asteraceae family, and include around 30 species including the rose of India and the marigold.

Said at least one pigment derived from a plant extract may be in pure form, or in the form of a product which is an oleoresin derived from a plant or an oleoresin paste derived from a plant. The plant extract can also be supported by a pigment carrier.

Advantageously, the invention relates to an aforementioned pigmenting composition comprising at least one pigment obtained from an extract of marigolds, in particular on a vegetable pigment support, in particular a bagasse of marigold (s), and a matrix, said at least one pigment, or supported pigment, in particular pigment supported on bagasse, being dispersed in said matrix, said matrix being a crystalline matrix essentially consisting of hydrogenated fatty acids, in particular hydrogenated oil, and at least one support.

The support for the matrix is advantageously silica.

Advantageously, said at least one pigment derived from a tagete extract can be in pure form, or in a product which is a tagete oleoresin or a tagete oleoresin paste. Said at least one pigment derived from an extract of tagetes can also be supported by a support for the pigment.

Marigold oleoresin is an extract or isolate of marigold flowers, obtained by extraction with volatile organic solvents, or supercritical _{CO 2.} This extraction results in a concentrate of the volatile (aromas) and non-volatile compounds of marigolds (triglycerides, waxes, dyes of a lipid nature such as xanthophyll pigments and flavoring compounds).

A tagete oleoresin paste is a tagete oleoresin that has been saponified and then solidified by a specific process or a combination of specific processes such as, in particular, evapo-concentration, the addition of a solidifying agent, or passing through a press.

Advantageously, the invention relates to the aforementioned composition, said composition further comprising up to 0.5% of at least one antioxidant, the percentages being expressed by mass relative to the total mass of the composition.

In addition to the aforementioned compounds, the composition according to the invention may contain from 0% to 0.5% by mass relative to the total mass of the composition of at least one antioxidant agent. This means that the antioxidant can be present at 0%, 0.05%, 0.1%, 0.15%, 0.2%, 0.25%, 0.3%, 0.35%, 0.4%, 0.45% or 0.5% in mass relative to the total mass of the composition

Advantageous antioxidant compounds are eugenol, ascorbic acid, vitamin C, tocopherols or vitamin E, polyphenols such as extracts of grapes, chestnut tannins, thymol or thyme extract, or a mixture of those -this.

Advantageously, the invention relates to the aforementioned composition, said composition further comprising from 0 to 6% of at least one hardening agent, the percentages being expressed by mass relative to the total mass of the composition.

In addition to the aforementioned compounds, the composition according to the invention may contain from 0% to 6% by mass relative to the total mass of the composition of at least one hardening agent. This means that the hardening agent can be present at 0%, 0.5%, 1%, 1.5%, 2%, 2.5%, 3%, 3.5%, 4%, 4, 5%, 5%, 5.5%, or 6% by mass relative to the total mass of the composition.

Advantageous hardening agents are calcium sulfate (CaSO ₄ ), sodium sulfate (Na ₂ SO ₄ ), dicalcium phosphate (Ca (PO ₄ ) ₂ ), monocalcium phosphate (CaH ₄ P ₂ O ₈ ), sodium chloride (NaCl), calcium chloride (CaCl ₂ ), or a mixture of these.

Such hardening agents are used to harden the pigmenting composition to give it a dry and brittle appearance. This aspect is sought after in the composition of the invention because it is known that poultry appreciate a dry and brittle product better.

Also, in the context of a composition intended for poultry, it will be advantageous to add at least one of these advantageous hardening agents to the composition.

Advantageously, the invention relates to the aforementioned composition, said composition comprising:

- from 0.2 to 20% of at least one xanthophyll pigment,

- 30 to 50% hydrogenated fatty acids,

- from 10 to 35% of at least one support, and

- optionally from 0 to 0.5% of at least one antioxidant, and

- optionally from 0 to 6% of at least one hardening agent,

the percentages being expressed by mass relative to the total mass of the composition.

Even more advantageously, the invention relates to the above-mentioned composition, said composition comprising:

- from 20 to 60% by mass relative to the total mass of the composition of a product comprising at least one xanthophyll pigment, said at least one xanthophyll pigment representing from 1 to 30% by mass relative to the mass of said product comprising at least one xanthophyll pigment,

- from 30 to 50% by mass relative to the total mass of the composition of hydrogenated fatty acids, and

- from 10 to 35% by mass relative to the total mass of the composition of at least one support,

- optionally from 0 to 0.5% by mass relative to the total mass of the composition of at least one antioxidant, and

- optionally from 0 to 6% by mass relative to the total mass of the composition of at least one hardening agent.

In an advantageous embodiment, the product comprising at least one xanthophyll pigment is an extract of marigolds which provides the pigments. In particular, the product comprising at least one pigment can be a tagete oleoresin or a paste of this oleoresin.

Advantageously, it is an oleoresin of marigolds deposited on a natural vegetable or natural mineral support, in particular a natural vegetable support, in particular on bagasses of marigolds.

In another aspect, the invention relates to a food intended for the nutrition of farm animals comprising from 0.01% to 1% by mass of a pigmenting composition as defined above, the percentages being expressed by mass per relative to the total mass of the food.

In other words, the invention relates to a food intended for the nutrition of farm animals comprising from 0.01% to 1% by mass relative to the total mass of the food of a pigmenting composition, said composition pigmenting agent comprising by mass relative to the total mass of the composition:

- from 0.2 to 20% of at least one xanthophyll pigment,

- from 30 to 50% hydrogenated fatty acids, and

- from 10 to 35% of at least one support.

By “0.01% to 1%” is meant in the invention a proportion of 0.01%, 0.02%, 0.03%, 0.04%, 0.05%, 0.06%, 0.07%, 0.08%, 0.09%, 0.1%, 0.11%, 0.12%, 0.13%, 0.14%, 0.15%, 0.16%, 0.17%, 0.18%, 0.19%, 0.2%, 0.21%, 0.22%, 0.23%, 0.24%, 0.25%, 0.26%, 0.27%, 0.28%, 0.29%, 0.3%, 0.31%, 0.32%, 0.33%, 0.34%, 0.35%, 0.36%, 0.37%, 0.38%, 0.39%, 0.4%, 0.41%, 0.42%, 0.43%, 0.44%, 0.45%, 0.46%, 0.47%, 0.48%, 0.49%, 0.5%, 0.51%, 0.52%, 0.53%, 0.54%, 0.55%, 0.56%, 0.57%, 0.58%, 0.59%, 0.6%, 0.61%, 0.62%, 0.63%, 0.64%, 0.65%, 0.66%, 0.67%, 0.68%, 0.69%, 0.7%, 0.71%, 0.72%, 0.73%, 0.74%, 0.75%, 0.76%, 0.77%, 0.78%, 0.79%, 0.8%, 0.81%, 0.82%, 0.83%, 0.84%, 0.85%, 0.86%, 0.87%, 0.88%, 0.89%, 0.9%, 0.91%, 0.92%, 0.93%, 0.94%, 0.95%, 0.96%, 0.97%, 0.98%, 0.99% or 1% by mass relative to the total mass of the food.

In the context of a composition where the pigment is not pure, but added in the form of a product comprising at least one xanthophyll pigment, the aforementioned food comprises from 0.01% to 1% by mass relative to the total mass of the food of a pigmenting composition, said pigmenting composition comprising:

- from 20 to 60% by mass relative to the total mass of the composition of a product comprising at least one xanthophyll pigment, said at least one xanthophyll pigment representing from 1 to 30% by mass relative to the mass of said product comprising at least one xanthophyll pigment,

- from 30 to 50% by mass relative to the total mass of the composition of hydrogenated fatty acids, and

- from 10 to 35% by mass relative to the total mass of the composition of at least one support.

Even more advantageously, the aforementioned food comprises from 0.01% to 1% by mass relative to the total mass of the food of a pigmenting composition, said pigmenting composition comprising by mass relative to the total mass of the composition :

- from 0.2 to 20% of at least one xanthophyll pigment,

- 30 to 50% hydrogenated fatty acids,

- from 10 to 35% of at least one support, and

- optionally from 0 to 0.5% of at least one antioxidant, and

- optionally from 0 to 6% of at least one hardening agent.

Even more advantageously, the aforementioned food comprises from 0.01% to 1% by mass relative to the total mass of the food of a pigmenting composition, said pigmenting composition comprising:

- from 20 to 60% by mass relative to the total mass of the composition of a product comprising at least one xanthophyll pigment, said at least one xanthophyll pigment representing from 1 to 30% by mass relative to the mass of said product comprising at least one xanthophyll pigment,

- from 30 to 50% by mass relative to the total mass of the composition of hydrogenated fatty acids, and

- from 10 to 35% by mass relative to the total mass of the composition of at least one support, and

- optionally from 0 to 0.5% by mass relative to the total mass of the composition of at least one antioxidant, and

- optionally from 0 to 6% by mass relative to the total mass of the composition of at least one hardening agent.

In another aspect, the invention relates to a process for preparing a composition as defined above, the process comprising the following steps:

a) contacting one or more hydrogenated fatty acids having a melting point of 35 ° C to 80 ° C, in particular hydrogenated oil having a melting point of 35 ° C to 80 ° C, with at at least one xanthophyll pigment and at least one support, said one or more hydrogenated fatty acids being brought to a temperature at least equal to the melting point of said one or more hydrogenated fatty acids so that the latter or these are in liquid or pasty form ,

b) the mixture, in particular homogeneous, of the compounds brought into contact in the preceding step, this step taking place for a sufficient time interval for the temperature of the mixture resulting from said mixture, in particular homogeneous, to drop to a temperature below the crystallization temperature of said one or more hydrogenated fatty acids to obtain a crystalline matrix essentially consisting of one or more hydrogenated fatty acids and at least one support, matrix in which said at least one xanthophyll pigment is dispersed.

Advantageously, the invention relates to the process for preparing a composition as defined above, the process comprising the following steps:

a) contacting one or more hydrogenated fatty acids having a melting point of 35 ° C to 80 ° C, in particular hydrogenated oil having a melting point of 35 ° C to 80 ° C, with at at least one tagete extract, possibly supported on bagasse, and at least one support, in particular silica, said one or more hydrogenated fatty acids being brought to a temperature at least equal to the melting point of said one or more hydrogenated fatty acids of so that this or these are in liquid or pasty form,

b) the mixture, in particular homogeneous, of the compounds brought into contact in the preceding step, this step taking place for a sufficient time interval for the temperature of the mixture resulting from said mixture, in particular homogeneous, to drop to a temperature below the crystallization temperature of said one or more hydrogenated fatty acids to obtain a crystalline matrix essentially consisting of one or more hydrogenated fatty acids and at least one support, matrix in which said at least one tagete extract is dispersed, possibly supported on bagasse .

The composition according to the invention is therefore prepared according to a simple process taking advantage of the crystallization properties of fatty acids or lipids and their melting and crystallization temperature.

In the invention, by "the homogeneous mixture" is meant the action of mixing the various constituents of the composition so that they are distributed in a quasi-uniform or uniform manner with respect to one another.

In order to produce the composition according to the invention, said one or more hydrogenated fatty acids, or hydrogenated lipids, are heated to a temperature going beyond the melting point (melting point) of the fatty acid (s), or lipids, as defined above. Said fatty acid, or said fatty acids, or lipids, are then in liquid form or in pasty form.

It is then possible to add the active compounds (said at least one pigment) to the fatty acids or lipids in liquid or pasty form. In order to achieve a uniform dispersion or not, the fatty acid / support / pigment mixture is mixed by any mixing or mixing means (pestles, spatulas, blades, screws, rotors, propellers, etc.). The temperature of the mixture, and in particular the temperature of the fatty acid (s), will then gradually decrease until it first drops below the melting point of the molten fatty acids. If the mixture is still stirred (or subjected to mixing), the temperature will decrease below the crystallization point of said fatty acid (s), thus inducing crystallization of this or these fatty acids.

It is thus, by gradual cooling with stirring, that the hydrogenated fatty acid (s) will gradually crystallize and, due to stirring, form crystals in the middle of which said at least one pigment and said at least one support will be finely dispersed, homogeneously or not.

The melting and crystallization temperatures of the advantageous oils are described above.

For example, a composition according to the invention made from refined and hydrogenated rapeseed oil will be obtained according to the following process:

The hydrogenated and refined rapeseed oil is heated to a temperature above 68 ° C (melting point) to obtain a liquid oil.

Pigments in the form of a product comprising at least one xanthophyll pigment and carrier, eg silica, premixed at room temperature, are added to the liquid oil, and the mixture is stirred.

Stirring is carried out for a time sufficient for the temperature of the mixture to reach a temperature below 49 ° C (crystallization temperature) in order to allow slow and gradual crystallization.

At the end of the process, crystals of refined and hydrogenated rapeseed oil have formed and said at least one pigment and said at least one support are found dispersed homogeneously or not between the crystals.

The mixing can be carried out by a conventional mixer known to those skilled in the art.

If the composition comprises additional compounds (for example an antioxidant, a hardening agent ...), these compounds are added to the molten fatty acids or in pasty form, at the same time as the pigment and the support.

The invention also relates to a composition comprising at least one xanthophyll pigment dispersed homogeneously or not in a crystalline matrix essentially consisting of one or more hydrogenated fatty acids and a support as defined above, said composition being capable of to be obtained, or obtained directly, by the aforementioned process.

The concentration of natural pigments (total xanthophylls) in the finished product is between 180,000 mg / kg and 2,000 mg / kg.

The invention finally relates to the use of a composition as defined above, or the food as defined above, for the yellow pigmentation of the flesh, legs or skin of poultry, in particular of poultry. poultry for breeding, or for pigmentation of the yolk of eggs of said poultry.

The level of yellow pigmentation of the flesh, legs or skin of poultry or the eggs of said poultry, or its variation (darker shade when the poultry have consumed the composition or the feed according to the invention) can be evaluated. according to two complementary methods, namely subjective colorimetry measurements (use of fans, scales or color charts of reference, recognized by those skilled in the art) or objective colorimetry measurements (use of a colorimeter, d 'chromameter or spectrophotometer).

With regard to subjective colorimetry measurements, pigmentation is assessed by a visual scoring of 1 to 15 (which correspond to increasing intensities of coloring) by one or more observers using a fan, a scale or a standard color chart making reference in the field of breeding and slaughter. These tools can be constructed specifically for scoring the yellowness of egg yolks, or specifically for scoring the yellowing pigmentation of chickens. A score of 1 denotes a very pale yellow and a score of 15 denotes a very pronounced orange-yellow color.

This yellow pigmentation can also be measured objectively using measuring tools calibrated and calibrated according to the international color system of the Hunter color space (Commission Internationale de l'Eclairage (CIE) - 1976): luminosity or clarity (L), red (a) and yellow (b), such as a colorimeter or chromameter (reflectance analysis). These tools are used to calculate the CIE 1976 L * a * b * color space, the hue (h * ab) and the luminous intensity (C * ab) of the color of yellow. L * ranges from 0 for black to 100 for white, a * ranges from -60 for green to +60 for red, and b * ranges from -60 for blue to +60 for yellow.

Advantageously, those skilled in the art will compare these two types of methods for measuring the yellow pigmentation.

This also means that the invention relates to a method for the yellow pigmentation of the flesh, legs or skin of poultry, in particular farmed poultry, or for the pigmentation of the yolk of the eggs of said poultry, comprising a step of administration, in particular by the oral route, to poultry, of a composition or of a food as defined above.

The method can also comprise a step of measuring the pigmentation either of the flesh, legs or skin of the poultry, or of the yolk of the eggs laid by said poultry.

The invention will be better understood thanks to the examples and figures which follow.

Brief description of the figures

The represents a graph showing the study of the stability over time of compositions comprising marigold pigments, under accelerated storage conditions (40 ° C. and 75% relative humidity). A represents Control 1, B, Control 2, C, the OLEO Cap A composition, and D, the OLEO Cap C composition. The Y axis represents the level of pigments expressed in percent relative to a base 100 at t0 , and the x-axis represents the time expressed in days.

The represents a graph showing the study of the stability over time of compositions comprising pigments of marigolds incorporated into poultry feed, under accelerated storage conditions (40 ° C. and 75% relative humidity). A represents control 1, B, control 2, C, the OLEO Cap composition A, D, the OLEO Cap C composition, and E, the control 3. The Y axis represents the level of pigments expressed as a percentage relative to at a base 100 at t0, and the x-axis represents time expressed in days.

The is a graph showing the visual pigmentation score (average DCF score) of chicken carcasses having consumed A: a feed without xanthophyll pigment, B: a feed comprising a commercial composition comprising tagete pigments in a synthetic matrix, C: a feed comprising the composition according to formula Test 1, D: a food comprising the composition according to formula Test 2, and E: a food comprising a commercial composition comprising marigold pigments on a natural plant support (tagète bagasse).

EXAMPLES Example 1: stability of pigments

The inventors first prepared two compositions according to the invention, with formulas mentioned in Table 1 below:

Formulas	OLEO Cap A		OLEO Cap C
Ingredients	%	kg	%	kg
Silica support	29.9	2,392	25	2
Hydrogenated palm oil	40	3.2	40	3.2
Eugenol	0.1	0.008	0.1	0.008
Calcium Sulphate	0	0	4.9	0.392
Pigments	30	2.4	30	2.4
qsp fluidifying	qsp 100	qsp 8	qsp 100	qsp 8
Total formula	100	8	100	8

The pigment is provided by a marigold oleoresin paste, the paste being standardized to 100 g / kg, or 100,000 ppm of pigments. During the analysis of this ingredient derived from marigold, the inventors however obtained a concentration of 78,000 ppm of pigments, which is slightly lower than the announced standard (an accuracy of +/- 20% is conventionally observed on this type of pigments. dosage).

After preparation of the compositions according to the process as described above, the level of pigments in each composition was assayed (D0).

First of all, the two products OLEO Cap A and OLEO Cap C both have an inclusion rate of 100%, the inclusion rate being the ratio between the pigments introduced into the formula and the pigments found in the matrix. finished. An inclusion rate of 100% means that all of the pigments introduced are found in the finished matrix, that is to say that there is no loss or degradation of the pigments during the process.

On the basis of these two compositions, the inventors tested the stability of the pigments as a function of time, by modeling ambient storage in commercial bags under accelerated conditions. To do this, they kept the different products at 40 ° C and 75% relative humidity. Under these conditions, a period of time determined under these experimental conditions corresponds to 3 times this time under ambient storage conditions (usual storage conditions).

The inventors compared the 2 OLEO Cap formulas described above with commercial products, namely:

- Control 1: a commercial composition comprising natural xanthophyll pigments (extracts of tagetes) encapsulated by “ spray drying ” with a synthetic polymer matrix,

- Control 2: a commercial composition comprising natural xanthophyll pigments (extracts of marigolds) sprayed on calcium carbonate, and a synthetic antioxidant (ethoxyquin), and

- Control 3: a commercial composition comprising natural xanthophyll pigments (extracts of tagetes) deposited on a natural plant support (tagète bagasse).

The stability of the pigments of the compositions alone, or of the pigments when the composition is incorporated into a feed for poultry, was tested at 30 days (D30) and 120 days (D120).

The results are shown in Figures 1 and 2.

Figures 1 and 2 highlight:

i) equivalent stability of the pigmenting composition according to the invention to that of control 1 (A) (a natural pigment encapsulated in a synthetic matrix), both for the finished product alone or incorporated in the feed intended for poultry.

ii) improved stability of the pigmenting composition according to the invention compared to that of control 2 (B) (a natural pigment on a calcium carbonate support with a synthetic antioxidant), both for the finished product alone or incorporated into feed for poultry.

iii) improved stability of the pigmenting composition according to the invention compared to that of control 3 (E) (a natural pigment on a plant support), at least for the finished product incorporated in the feed intended for poultry (the data on finished product alone not available).

These results show that a pigment whether placed on a calcium carbonate support or a plant support will be less stable over time, including with an addition of antioxidant, compared to a pigment protected by a matrix (matrix composed of hydrogenated vegetable oil and a support) such as the composition according to the invention or a synthetic matrix.

Example 2: coloring tests on broilers

In a second test, the inventors tested in vivo the tinting power of two compositions according to the invention, in comparison with that of a negative control not comprising pigment (mixture of middlings of wheat, calcium carbonate and semolite sepiolite) , and those of two positive controls, the commercial compositions corresponding to Controls 1 and 3 of Example 1.

The test was carried out in an experimental station: 780 chickens were allotted at 0 days at the rate of 39 male Ross 308 chickens per 2.6 m² floor, divided into 5 groups of 4 floors, or 156 chickens per group.

The batching was made according to the average weight per floor on arrival. The density of animals in conventional breeding conditions of 15 animals per m² is respected.

The trial lasted 35 days after which some animals were slaughtered (32 animals per group, 2.7 kg live weight on average).

The compositions according to the invention tested (Test 1 and Test 2 formulas) are manufactured according to the formulas mentioned in Table 2 below:

	Formula 1 test	Formula Test 2
Silica support	27.3%	25%
Eugenol	0.1%	0.1%
Calcium Sulphate	4.9%	4.9%
Hydrogenated palm oil	33.1%	31.5%
Pigment	25.9%	29%
Fluidifying	8.7%	9.5%
Total formula	100%	100

As in Example 1, the pigment is provided in these 2 compositions according to the invention by a marigold oleoresin paste (same characteristics).

Each of the compositions (commercial and according to the invention) is first incorporated into a premix (PM) according to the compositions mentioned in Table 3 below:

	PM White Witness neg.	PM Witness 1	PM Witness 3	PM Trial 1	PM Trial 2
Sepiolitis semoulette	35%	34%	26%	30%	30%
Hydrogenated palm oil	55%	53%	41.25%	47%	47%
Pigments	10%	9.5 %%	7.5%	8%	8%
Witness 1	-	3.5%	-	-	-
Witness 3	-	-	25%	-	-
Form Test 1	-	-	-	14%	-
Formula Test 2	-	-	-	-	14%
Total PM	100%	100%	100%	100%	100%
PM incorporation rate in food:

• Start-up

1% 0.34% 0.31% 0.31% 0.27%

• Growth

2% 0.97% 0.89% 0.90% 0.76%

• Finishing

2.5% 1.39% 1.28% 1.29% 1.08%

The food program is the same for the 5 groups. The feeds are formulated to meet the nutritional needs of broilers. Maize and maize by-products are prohibited in the formulation of these foods, to avoid coloring bias.

Nutritional constraints are conventional, apart from a constraint in expected yellowing power varying from 10 to 35 ppm depending on the phases, and another constraint in expected blushing capacity varying from 1 to 3 ppm. These constraints are identical for all the Control and Test groups.

The rate of incorporation of the above premixes is therefore variable according to the phases (Start-up, Growth, Finishing) and the Control and Test groups, to meet the constraints imposed on the yellowing and reddening powers, namely (Yellow power / Red power in ppm): Starting (10.01 / 1), Growth (25/2) and Finishing (35/3). The incorporation rates of each of the premixes according to the different phases of the test are specified in Table 3 above.

Measures :

In addition to measurements on the animal on the farm to ensure the proper conduct of the test in terms of zootechnical performance and animal welfare (Average Daily Gain, Weight, Consumption Index, Water consumption , Bedding note, follow-up of lesions on the legs and breasts), measurements on the level of coloring of the carcasses of the animals were carried out:

• on D21, objective pigmentation measurements (Minolta chromameter) are carried out on the legs of 6 animals per floor. A visual notation is also carried out (scale from 1 to 15, colorimetric range DSM).
• on D35, 160 chickens are slaughtered, ie 32 animals per group, chosen from among the most representative animals in the average weight of their floor. Pigmentation measurements are taken on the back, thighs and fillets of each slaughtered animal by objective measurement (Minolta chromameter) and visual scoring (scale from 1 to 15, DSM colorimetric range). Two average scores, one objective and one visual, are calculated for each individual: DCF scores (for back, thighs, fillets).

Results:

Few significant variations were observed between the control groups and the two compositions according to the invention in zootechnical performance, over the duration of the test.

Regarding the pigmentation performance, the objective measurements (Minolta chromameter) carried out on D35 show that:

Brightness L *: The Test 1 and 2 and Control 1 groups have an L * similar to the Negative Control group. The Control 3 group has significantly lower luminance than the Negative Control group.

Red a *: Control groups 1 and 2 have a significantly lower a * than the negative control group, over the entire carcass (back / thigh / tenderloin). The Test 1 and 2 groups have as much red as the Negative Control group (slightly lower numerically but not statistically significant difference).

Yellow b *: The Negative Control group is the group with the least yellow, it is significantly less yellow than all the other groups (p <5%). Positive Control groups 1 and 2 are the groups with the most yellow. The Test 1 and 2 groups are intermediate, between the Negative Control group and the Positive Control 1 and 2 groups.

The results of the visual scoring at D35 are presented in the . We observe that:

• The highest DSM rating was obtained with Control group 1 (a natural pigment encapsulated in a synthetic matrix)
• The Test 1 and Test 2 formulas have intermediate DSM scores at Negative Control and Positive Controls 1 and 2.

Conclusion:

These results show that a pigment protected by a matrix (consisting of vegetable oil with a carrier) such as the composition according to the invention is bioavailable and allows significant coloring of the meat of broilers compared to a diet without pigment (negative control ), even if the coloration obtained is lower than that obtained with a pigment protected by a synthetic matrix or a pigment placed on a plant support.

These results are very encouraging, because the chain of production and consumption of poultry meat and eggs (from the breeder to the consumer, including slaughterhouses) will turn to a composition according to the invention, meeting the expectations of stability. and naturalness, while guaranteeing a widely acceptable coloring power.

Example 3: Complementary study of the stability of pigments on a support

In addition to Example 1, the inventors tested other compositions in order to evaluate the stability over time of a pigment on a support. The conditions of Example 1 have been implemented.

The following compositions were prepared:

	COLOR1	COLOR4	COLOR5	COLOR6
Ingredients	%	%	%	%
Silica support	10	12.5	12.5	12.5
Hydrogenated oil	50 Palm oil	50 Palm oil	50 Palm oil	50 Sunflower oil
Vitamin C	0	0.5	1	0
Calcium sulphate	3.5%	3	2.5	3.5
Product comprising a xanthophyll pigment	36.5 Tagète extract on bagasse (including 1.5% pigment)	34 Tagète extract on bagasse (including 1.5% pigment)	34 Tagète extract on bagasse (including 1.5% pigment)	34 Tagète extract on bagasse (including 1.5% pigment)
Total	100	100	100	100
	COLOR10	COLOR11	COLOR13	COLOR14
Ingredients	%	%	%	%
Silica support	10	12.5	12.5	12.5
Hydrogenated oil	50 Palm oil	50 Palm oil	50 Palm oil	50 Sunflower oil
Vitamin C	0	0	0.5	1
Calcium Sulphate	3.5	3.5	3	2.5
Product comprising a xanthophyll pigment	36.5 Marigold extract on calcium carbonate (including 6% pigment)	34 Marigold extract on calcium carbonate (including 6% pigment)	34 Marigold extract on calcium carbonate (including 6% pigment)	34 Marigold extract on calcium carbonate (including 6% pigment)
Total	100	100	100	100
	COLOR Inv control	COLOR control Calcium carbonate	COLOR Synthesis control
Ingredients	%	%	%
Silica support	0	0	0
Hydrogenated oil	0	0	0
Vitamin C	0	0	0
Calcium Sulphate	0	0	0
Product comprising a xanthophyll pigment	100 Tagète extract on bagasse (including 1.5% pigment)	100 Marigold extract on calcium carbonate (including 6% pigment)	100 Marigold extract not supported in a synthetic matrix (including 10% pigment)
Total	100	100	100

The compositions COLOR1, 4, 5, 6 and COLOR Inv comprise as pigment extracts of tagetes on a plant support, which support is tagète bagasse. Note that, unlike the COLOR1, 4, 5, 6 compositions, the COLOR Inv control is not dispersed in a matrix of hydrogenated vegetable oil with a support.

The compositions COLOR10, 11, 13, 14 and COLOR Calcium carbonate, for their part, comprise extracts of marigolds deposited on a calcium carbonate support. Note that, unlike the COLOR10, 11, 13, 14 compositions, the COLOR calcium carbonate control is not dispersed in a matrix of hydrogenated vegetable oil with a carrier.

The COLOR Synthesis control for its part comprises extracts of unsupported marigolds, encapsulated by “spray drying” with a synthetic polymer matrix (commercial composition).

The stability of the pigments within the various aforementioned compositions was measured at 90 days and at 150 days after setting under the above-mentioned conditions (40 ° C., 75% humidity).

The results are presented in the following table in the form of the percentage change in the pigment content relative to the pigment content used at the start of the experiment.

	J90 deviation	J150 deviation
COLOR1	-3%	-5%
COLOR4 ***	-13%	-14%
COLOR5	nd	-1%
COLOR6	0%	-6%
COLOR10	-37%	nd
COLOR11	-37%	nd
COLOR13	-33%	nd
COLOR14	-30%	-45%
COLOR Synthesis	-15%	-27%
COLOR Inv	-5%	-14%
COLOR Calcium carbonate	-67%	nd

nd: measurement not carried out.

The threshold of analytical significance of the reduction in the pigment content is fixed at -15% whether it is at 90 days or 150 days.

Regarding the controls, these results show that:

- placing a vegetable pigment on a calcium carbonate support (COLOR Calcium carbonate) does not make it possible to maintain the stability of the pigments from 90 days, and

- placing an unprotected pigment on a bagasse support (without a matrix of hydrogenated vegetable oil with support) (COLOR Inv) allows better maintenance of the stability of the pigment compared to an encapsulation of the pigment in a synthetic matrix (COLOR Synthesis) .

It should also be noted that the protection in a matrix of hydrogenated oil with a carrier (palm oil or sunflower oil) of the plant pigment on a calcium carbonate carrier (COLOR 10, 11, 13 and 14) does not make it possible to maintain the stability of the pigments at 150 days, although the stability is improved compared to the pigment sprayed on calcium carbonate without a hydrogenated oil matrix with support (COLOR Calcium carbonate). A pigment deposited on calcium carbonate, the whole being included in a matrix composed of hydrogenated vegetable oil and a support, is therefore not compatible with the imposed stability conditions (less than -15% at 150 days or even at 90j).

Regarding the compositions according to the invention COLOR1, 4, 5 and 6, it will be noted that whatever the composition (presence or absence of vitamin C) and whatever the hydrogenated oil used (palm or sunflower), a better stability at 150 days compared to the COLOR Inv control, and therefore to the commercial pigment composition in a synthetic matrix (COLOR Synthesis) as shown above.

*** The COLOR 4 composition behaves a little differently due to poorer incorporation of the pigment during preparation.

All of these results show that the compositions according to the invention COLOR1, 4, 5 and 6 therefore have improved stability compared to

- to a benchmark commercial composition (COLOR synthesis), and

- to a pigment that is not protected in a matrix (vegetable oil and carrier) (COLOR Inv).

This improved stability makes the prolonged storage of these compositions according to the invention more effective than the other compositions described above.

Example 4: coloring tests on laying hens

In a new test, the inventors tested in vivo the coloring power of a composition according to the invention (COLOR6 of Example 3), in comparison with that of a negative control without any contribution of yellow pigment (T-). , a positive control comprising a synthetic yellow commercial pigment (T +), and a control (extract of tagetes on a non-vectorized bagasse support - COLOR Inv of Example 3).

The test was carried out in an experimental station: 200 laying hens were allotted at 41 weeks of age at the rate of 2 hens per box, i.e. 750 cm² / animal, the hens being divided into 12 groups of 8 or 9 boxes, i.e. 16 or 18 animals per group.

The batching was defined based in particular on the average weight per egg, the rate of downgraded eggs and the general condition of the animals (visual assessment).

The trial lasted 6 weeks, including 3 weeks of adaptation followed by 3 weeks of testing itself.

Throughout the test, the animals are fed feed formulated to meet the conventional nutritional requirements of laying hens. Maize and maize by-products (gluten, spent grains) are prohibited in the formulation of these foods to avoid color bias.

During the adaptation phase (21 ^st days), all the animals are fed with a control food without pigment.

Then, from the 22 ^th day, and during the 20 days, yellow pigmenting compositions (color6, COLOR Inv or T +) are added to test food.

The animals of the T- group receive the same food without the addition of yellow pigment.

All the animals receive the same dose of natural red pigment (commercial composition) so as to reproduce the pigmentation strategies observed in the field and so as to be able to rule only on the yellow pigment effect.

The composition according to the invention (COLOR6) and the control composition (COLOR Inv) are tested at 5 increasing doses of incorporation into the food (dose-response), ie 5 groups of animals for each of the compositions tested.

The rates of incorporation of each of the pigmenting compositions in foods are specified in the table above.

	T-	T +	COLOR Inv D1	COLOR Inv D2
Nature contribution yellow pigment	/	synthetic commercial yellow pigment	COLOR Inv	COLOR Inv
Nature red pigment supply	natural red commercial pigment	natural red commercial pigment	natural red commercial pigment	natural red commercial pigment
Yellowing power (ppm)	0.34	10	5	10
Incorporation rate of the yellow pigment in the food (%)	0%	0.0039% (of the composition comprising 10% pigment)	0.0452% (of the composition comprising 1.5% pigment)	0.0936% (of the composition comprising 1.5% pigment)
	COLOR Inv D3	COLOR Inv D4	COLOR Inv D5	COLOR6 D1
Yellow pigment contribution	COLOR Inv	COLOR Inv	COLOR Inv	COLOR 6
Red pigment contribution	natural red commercial pigment	natural red commercial pigment	natural red commercial pigment	natural red commercial pigment
Yellowing power (ppm)	15	20	25	5
Feed intake rate	0.1421% (of the composition comprising 1.5% pigment)	0.1905% (of the composition comprising 1.5% pigment)	0.2390% (of the composition comprising 1.5% pigment)	0.1192% (of the composition comprising 0.57% pigment)
	COLOR6 D2	COLOR6 D3	COLOR6 D4	COLOR6 D5
Yellow pigment contribution	COLOR 6	COLOR 6	COLOR 6	COLOR 6
Red pigment contribution	natural red commercial pigment	natural red commercial pigment	natural red commercial pigment	natural red commercial pigment
Yellowing power (ppm)	10	15	20	25
Feed intake rate (%)	0.2470% (of the composition comprising 0.57% pigment)	0.3749% (of the composition comprising 0.57% pigment)	0.5027% (of the composition comprising 0.57% pigment)	0.6305% (of the composition comprising 0.57% pigment)

The yellowing power reflects the effectiveness of the food's yellow pigmentation. It is based on the pigmentation efficiency of each feed material, taking into account their stability and bioavailability. It is also a function of the level of fat present in the food (which can positively influence the bioavailability of pigments). It is expressed in parts per million and is defined according to the species (here, "spawn").

Measures :

In addition to measurements on the animal on the farm to ensure the proper conduct of the test in terms of zootechnical performance (feed consumption per cage, number of eggs laid, average egg weight, visual classification eggs: broken, pitted, soft and dirty, mortalities, morbidities), the following measurements on the level of coloring of the eggs were carried out:

• 3 eggs per cage (ie 300 eggs in total) are collected and identified during the last 4 or 5 days of the test. Each egg is weighed with the shell, then broken. The yellow pigmentation is visually assessed with the DSM scale and measured with the Minolta (model CR 400); and
• 5 egg yolks per group are selected and pooled during the last 4 or 5 days of the test, in order to determine the lutein in the egg. Lutein determined after dissolving in water, followed by extraction with ethanol and methanolic potash. This extraction is then followed by a triple extraction with ether, in ampoules. After evaporation of the ether, and change of solvent, the lutein is analyzed by HPLC-UV.

Claims (10)

1. Pigmenting composition comprising at least one xanthophyll pigment, and a matrix, said at least one xanthophyll pigment being dispersed in said matrix, said matrix being a crystalline matrix essentially consisting of hydrogenated fatty acids, in particular hydrogenated oil, and at minus a support.
2. Composition according to Claim 1, comprising by mass relative to the total mass of the composition:
   - from 0.2 to 20% of at least one xanthophyll pigment
   - from 30% to 50% hydrogenated fatty acids, and
   - from 10 to 35% of at least one support.
3. A composition according to claim 1 or claim 2, wherein said at least one xanthophyll pigment is at least one of the following pigments: lutein, zeaxanthin, beta-carotene and capsanthin.
4. Composition according to any one of the preceding claims, wherein said at least one pigment is obtained from a plant extract, in particular from an extract of marigold.
5. Composition according to any one of the preceding claims, said composition further comprising up to 0.5% of at least one antioxidant, the percentages being expressed by mass relative to the total mass of the composition.
6. Composition according to any one of the preceding claims, comprising from 0 to 6% of at least one hardening agent, the percentages being expressed by mass relative to the total mass of the composition.
7. Composition according to any one of the preceding claims, comprising:
   - from 0.2 to 20% of at least one xanthophyll pigment,
   - from 30 to 50% hydrogenated fatty acids,
   - from 10 to 35% of at least one support,
   - from 0 to 0.5% of at least one antioxidant, and
   - from 0 to 6% of at least one hardening agent,
   the percentages being expressed by mass relative to the total mass of the composition.
8. Food intended for the nutrition of farm animals comprising from 0.01% to 1% by mass of a pigmenting composition as defined in any one of claims 1 to 7, the percentages being expressed by mass relative to the total mass of the food.
9. Process for preparing a composition according to any one of claims 1 to 7 comprising the following steps:
   a) contacting one or more hydrogenated fatty acids having a melting point of 35 ° C to 80 ° C, in particular hydrogenated oil having a melting point of 35 ° C to 80 ° C, with at at least one xanthophyll pigment and at least one support, said one or more hydrogenated fatty acids being brought to a temperature at least equal to the melting point of said one or more hydrogenated fatty acids so that the latter or these are in liquid or pasty form ,
   b) the mixture, in particular homogeneous, of the compounds brought into contact in the preceding step, this step taking place for a sufficient time interval for the temperature of the mixture resulting from said mixture, in particular homogeneous, to drop to a temperature below the crystallization temperature of said one or more hydrogenated fatty acids to obtain a crystalline matrix essentially consisting of one or more hydrogenated fatty acids and at least one support, matrix in which said at least one xanthophyll pigment is dispersed.
10. Use of a composition as defined in any one of Claims 1 to 7, for the yellow pigmentation of the flesh, legs or skin of poultry, in particular of farmed poultry, or for the pigmentation of the yolk eggs of said poultry.

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