Method for obtaining a vitamin k3-enriched powdered milk for puppies and kittens

Abstract

The invention relates to the field of nutritional compositions for young animals, such as milk with a high vitamin content for puppies and kittens. More particularly, the invention relates to a method for obtaining a milk-type nutritional composition characterised by a high vitamin K3 content.

Description

PROCESS FOR OBTAINING POWDERED MILK FOR PUPPIES AND KITTENS ENRICHED WITH VITAMIN K3 The invention relates to the field of nutritional compositions with a high vitamin content for young animals, such as milk for puppies and kittens. More particularly, the invention relates to a method for obtaining a nutritional composition of the powdered milk type, having the characteristic of a high vitamin K3 content, this vitamin K3 being in the MNB form. Field of invention In animal nutrition, it is beneficial to have high-nutritional value compositions. Young animals, such as kittens and puppies, in particular, often require vitamin supplementation. It is common for this supplementation to be provided through food, so as to provide all the vitamins and minerals necessary for the animal's health in a simple and inexpensive manner. Vitamin K3, or menadione, is a synthetic form of active vitamin K precursor (biochemically converted into active vitamin K in the body). This vitamin plays an important role in the health of pets, particularly in blood clotting. Vitamin K3, commonly added to pellets, is unstable. Sensitive to light and heat, this vitamin is also affected by interactions with choline. As a result, its incorporation into an animal milk preparation process does not produce milk with a high vitamin K3 content. Vitamin compositions for animals containing vitamin K3 are known from the state of the art. Document EP1265496 describes a liquid vitamin composition composed of (a) a first liquid vitamin preparation comprising vitamins A, D3, B12 and optionally vitamin E, (b) a second liquid vitamin preparation containing vitamins B1, B2, B3, B5, B6 and H, and finally (c) a third liquid vitamin preparation comprising vitamin K3. The three preparations of the composition described are separate solutions. Document CN112753864 describes a liquid vitamin compound, which belongs to the field of animal feed. The liquid vitamin compound is prepared from the following components: vitamin A, vitamin D3, vitamin E, vitamin K3, vitamin B, oligosaccharide, an antioxidant, calcium lactate, polyglycerol ricinoleate and a carrier. It is also known from the prior art to obtain vitamin K3 derivatives. Document EP2461699 describes vitamin K3-derived particles formulated with highly stabilized nicotinamide (NA). The NA forms a physical protective layer (both continuous and discontinuous) leading to the production of highly stabilized vitamin K3-derived particles (MNB form). The prior art also includes sprayable vitamin compositions. Documents CN101874571 and CN101874572 describe sprayed vitamin compositions on the surface of a cat or dog food and a spraying method thereof. The vitamin composition further comprises vitamin K3. The spraying method comprises the following main steps: preparing a base material and the vitamin composition, then spraying the vitamin composition on the surface of the base material by counter-blowing, and finally cooling and packaging to obtain the finished product. Document EP0385335B1 describes a stabilized vitamin K composition. This composition comprises at least 0.017% by weight of vitamin K based on the total weight of the composition and at least 0.01% by weight, based on the weight of the vitamin composition, of stabilizer selected from the group consisting of β-carotene, γ-carotene, lycopene and canthaxanthin (

[0005] ). Vitamin K may be vitamin K3 (

[0010] ). Said composition is obtained according to the following steps: dissolving liposobule vitamin K in an oily component and then adding a stabilizing amount of specified carotenoids. Emulsifiers, such as egg yolk phospholipids, may be added as solubilizing agents depending on the intended purpose. US3196018A, CN110301543A and US3079260A describe veterinary feed compositions comprising vitamin K3 in the form of menadione sodium bisulfite (MSB). The Anonymous document: "How Lecithin Improves the Production of Milk Powder?", describes the role of sprayable or liquid lecithin in the solubility of a powdered product. Finally, document EP0385335B1 describes a milk powder for guinea pigs as well as its preparation process and its application, intended to provide a feed suitable for the breeding of sterile guinea pigs. Said milk powder comprises by weight the following ingredients: 75 to 85 parts of soy protein; 115-125 parts of caseins; 4.5 to 5.5 parts of L-methionine; 300 to 330 parts of corn starch; 32 to 38 parts of maltodextrin; 335 to 365 parts of sucrose; 120 to 130 parts of cellulose; 22-28 parts of guar gum powder; 18-22 parts of lard; 22 to 28 parts of soybean oil; 72 to 78 parts of mineral premix; 9 to 11 parts of vitamin premix; 1.8 to 2.2 parts of choline bitartrate; guinea pig milk powder is sterilized.The process for obtaining said powder includes the following steps: the raw materials are transformed into powder, then mixed uniformly and placed in a sealed environment, pasteurized (water bath at 85 degrees Celsius for 20 minutes) and irradiated (irradiation with cobalt 60, dose 15 kgy). In addition, said powder includes vitamin K3 in MSB form. Double sterilization is then applied to obtain powdered milk for guinea pigs. Due to the instability of this vitamin, there is currently no nutritional composition suitable for feeding puppies and kittens, including a high content of vitamin K3 that remains stable, especially a few months after production. The inventors have developed a process for manufacturing a nutritional composition with a high vitamin K3 content in the form of milk powder, intended for feeding and maintaining the vitamin intake of young animals. The process includes parameters that have been tested and adjusted so as to guarantee a determined quantity of vitamin K3 in the resulting product for at least 24 months. The inventors have, in fact, developed a process whose parameters are optimized to limit the degradation of vitamin K3 during preparation, thus making it possible to obtain a composition with a high vitamin K3 content, namely a quantity greater than or equal to 1.5 mg / Kg of vitamin K3 for at least 18 months after production of said composition. The invention therefore relates to a process for obtaining a milk powder for young animals enriched with vitamin K3, characterized in that it comprises the following steps: (I) Subject the preparation tank, containing the ingredients suitable for producing animal milk and vitamin K3, to a heat treatment between 20 and 80°C to obtain a mixture; (II) Pasteurization of the mixture obtained in step (I) at a temperature between 70°C and 75°C; (III) Drying of the mixture obtained in step (II) during which a lecithination treatment is applied to said mixture; (IV) Collection of milk powder enriched with vitamin K3 at the end of step (III); wherein said vitamin K3 is in MNB form. A second subject of the invention relates to a milk powder suitable for feeding young animals such as puppies and kittens, characterized by a vitamin K3 content greater than or equal to 1.5 mg / kg for at least 18 months after the production of said powder. Advantages of the invention The present invention addresses an unmet need for a milk powder rich in vitamin K3, in particular with a quantity greater than or equal to 1.5 mg / kg of vitamin K3 for at least 18 months after the production of said powder and a nutritional composition suitable for young animals, such as puppies and kittens. The method according to the invention makes it possible to obtain a nutritional product that can be offered in pet stores and at veterinarians. In contrast, animal milks enriched with vitamin K3 available on the market mention a quantity of vitamin K3 at the time of formulation but no guarantee is provided on the evolution of this quantity over time. However, it is known that vitamin K3 is the most unstable type of vitamin. Vitamin K3 comes in two forms: menadione sodium bisulfite (MSB) and menadione nicotinamide bisulfite (MNB). Of these two forms, MNB vitamin K3 is more resistant and stable than MSB. However, MNB vitamin K3 is neither water-soluble nor fat-soluble, which poses formulation challenges. Vitamin K3 is therefore a vitamin whose addition is problematic during the milk production process. Indeed, on the one hand, the soluble form is labile, on the other, the resistant form is not water-soluble. In addition, this vitamin is sensitive to light, heat and is also affected by interactions with choline. The amount of vitamin K3 therefore tends to naturally decrease over time. For all these reasons, adding and maintaining a high amount of vitamin K3 in a composition poses formulation problems. The inventors have developed a process for obtaining milk powder optimized to limit the degradation of vitamin K3, by choosing to enrich this milk powder with vitamin K3 in MNB form. As a result, it is possible, thanks to the process of the present invention, to formulate compositions having a high vitamin K3 content that is stable for at least 24 months. This makes it possible to guarantee a high vitamin K3 content during the shelf life of the powdered milk, i.e. at least 18 months at room temperature (i.e. between 15 and 25°C). DETAILED DESCRIPTION OF THE INVENTION A first subject of the invention relates to a process for obtaining a milk powder for young animals enriched with vitamin K3, characterized in that it comprises the following steps: (I) Subject the preparation tank, containing the ingredients suitable for producing animal milk and vitamin K3, to a heat treatment between 20 and 80°C to obtain a mixture; (II) Pasteurization of the mixture at a temperature between 70°C and 75°C; (III) Drying of the mixture obtained in step (II) during which a lecithination treatment is applied to the mixture; (IV) Collection of milk powder enriched with vitamin K3 at the end of step (III); wherein said vitamin K3 is in MNB form. In a preferred embodiment, the amount of vitamin K3 present in step (I) is at least 4 mg / Kg of milk powder. Preferably, the amount of vitamin K3 is between 4 mg / Kg and 6 mg / Kg. By "milk powder" is meant a product obtained from ingredients of dairy origin in powder form. By "ingredients suitable for producing animal milk" is meant any ingredient that can allow the formulation of milk intended for animals. The ingredients for obtaining a mixture as considered in the invention may be, without being limited to: a dairy preparation containing, for example, milk proteins, fats, fibers, vitamins and minerals, amino acids, choline. “Vitamin K3” means any form of vitamin K3, such as, for example, menadione sodium bisulfite (MSB) or menadione nicotinamide bisulfite (MNB). “Vitamin K3 MNB” means menadione nicotinamide bisulfite or “vitamin K3 Menadione Nicotinamide Bisulfite”. In a preferred embodiment, the ingredients constituting the formulation are added directly into the preparation tank in step (I), the pH of the mixture in the preparation tank is neutral and has a temperature slightly higher than room temperature and the agitation of the tank during the treatment of the different ingredients is between 400 and 500 rpm. The preparation can be stored in the tank, at a temperature between 20-80°C for a period of up to 1 hour, at most 2 hours after the addition of vitamin K3 and before the pasteurization step. Vitamin K3 is the last ingredient added to maintain its stability. The inventors determined that adding vitamin K3 to the process before the drying step avoids the problems typically encountered when formulating with vitamin K3. In a preferred embodiment, the heat treatment of step (I) is carried out at a temperature between 40°C and 60°C, more particularly between 45 and 55°C. Pasteurization step (II) can be carried out at a temperature between 70°C and 75°C. This step will not be detailed further, as the person skilled in the art has the knowledge required to carry out pasteurization. Step (III) of drying the mixture can be carried out by any drying means conventionally used to obtain a milk powder. For example, this may involve freeze-drying, fluidized bed drying or hot air drying. The drying according to the invention can be carried out by spraying in a multi-stage MSD tower with dry air atomization. The drying includes lecithination of the mixture. This step is carried out by spraying soy lecithin simultaneously with the spraying of the milk preparation in the tower. This technique gives the powder good dispersibility and wettability properties. In a particular embodiment, the drying step (III) is carried out at inlet temperatures of between 235 and 245°C and outlet temperatures of between 75 and 85°C. The milk powder obtained is collected in step (IV). This milk powder can be stored by packaging in large capacity bags, in a storage area at room temperature. The milk powder according to the invention comprises a quantity of vitamin K3 greater than or equal to 1.5 mg / kg for at least 24 months after the production of said powder. This means that a minimum quantity of 1.5 mg / kg is present in the milk powder at 1 month, 6 months, 12 months, 18 months for example. The quantity of vitamin K3 present can for example be measured by chemical analysis by gas chromatography coupled with a mass spectrometer (GC / MS) or by liquid chromatography (LC / DAD). In a particular embodiment, the milk powder comprises between 1.5 and 10 mg / kg of vitamin K3 for at least 18 months, preferably at least 24 months after its production. In preferred embodiments, the milk powder comprises between 1.5 and 5 mg / kg, or even between 2 and 5 mg / kg for at least 18 months, preferably at least 24 months after its production. In particular embodiments, the milk powder comprises between: 2.5 and 10, or 3 and 10 or 4 and 10 or even 3 and 5 mg / kg of vitamin K3 powder, the amount of which is stable for at least 18 months, preferably 24 months after the production of said powder. Preferably, the vitamin K3 present in the milk powder is in MNB form (this characteristic combines with the value ranges described above). EXAMPLES EXAMPLE 1: Process for obtaining a milk powder according to the inventionMaterials and methods Vitamin K3 The vitamin K3 used is the bisulfite form of menadione nicotinamide (MNB). Fine, white to yellowish, free-flowing, micro-granular powder with complex characteristics. Preparation of vitamin K3 Vitamin K3 is weighed and stored in a pillbox and aluminum foil bag away from light before production. Preparation of the dairy matrix Dairy recipe composed of milk proteins, fats, fibers, vitamins and minerals, amino acids, choline. Sequence of preparation of the dairy preparation: - Preparation of a dairy base - Addition of fats with antioxidants - Addition of vitamin, mineral, fiber and amino acid premix including choline - Addition of vitamin C - Addition of vitamin K3 The pH of the recipe is between 6.7 and 7.0 at 40°C and is stored between 40-55°C before being pasteurized. The agitation of the tank during the processing of the various ingredients is carried out between 420 and 460 rpm. The preparation is stored in the tank for a maximum of 2 hours after adding vitamin K3 and before pasteurization. pasteurization stage A heat treatment is applied to the product before it is sprayed into the drying tower. The product is pasteurized between 71.8°C and 72.2°C. drying stage Drying is carried out in a multi-stage MSD tower with dry air atomization. The spraying of soy lecithin is carried out simultaneously with the spraying of the milk preparation in the tower. Conservation The powder is packaged in large capacity, non-gassed bags in a storage area at room temperature. Analytical interpretation Vitamin K3 analyses were performed in several laboratories depending on the progress of the project as well as the limit of quantification (LOQ).UPSCIENCE: LOQ 0.3 ppm = (A)EUROFINS: LOQ 1 ppm = (B)MERIEUX: LOQ 0.3 ppm = (C)Results Pilot tests and then industrial tests were then carried out before moving on to production. Pilot tests The pilot tests enabled the approach to be validated and the optimal value ranges for implementing the process to be determined. Industrial testing Industrial-scale tests have provided a better understanding of vitamin K3 losses during the process and have allowed us to determine the necessary dosage of raw materials. The results obtained are satisfactory, particularly with an initial quantity of vitamin K3 of 6 mg / kg of milk powder. The average loss is 70.35%. This loss is nuanced by the dilution of the product containing vitamin K3 by the product not containing vitamin K3, as the addition is not carried out on complete productions. This dosage makes it possible to find vitamin K3 in sufficient quantity with respect to the target defined in the finished product. Productions Table 1: Analytical results of vitamin K3 in the productions All results regarding vitamin K3 are consistent and homogeneous. We have an average loss of 54.72% in the process. The loss is lower than industrial tests because the addition of vitamin K3 was done on complete productions, without dilution. Conclusion Following the various tests on the addition of vitamin K3, all the process parameters as well as the formulations allowing the expected quantity to be obtained in the finished product were established. This example shows that it is possible to obtain milk powder containing a vitamin K3 content greater than 2.5 mg / kg in the finished product. The powder is then packaged in large capacity bags at room temperature. EXAMPLE 2: Study of the variation over time of the content of vitamin K3 MNB in ​​powdered milk for puppies and kittens. A stability study was conducted on vitamin K3 contained in powdered milk for puppies and kittens obtained according to the method of the present invention.Materials and Methods Materials and methods The powder was obtained following the same materials and methods as described in Example 1. The powder was stored in aluminum foil bags at room temperature for 18 months. Liquid chromatography (LC / DAD) analyses of vitamin K3 content (in mg / kg) were performed at the following times: 7 months, 9 months, 12 months, 15 months, and 18 months. Results The results are presented in Table 2 below:T0T+ 7 monthsT+ 9 monthsT+ 12 monthsT+ 15 monthsT+ 18 monthsVitamin K3 content in mg / KgAverage 2.833.0+ / -0.42.84+ / -0.573.73+ / -0.7462.33+ / -0.4663.13+ / -0.626 Table 2: Vitamin K3 results in powdered milk for puppies and kittens during 18 months of DDM study It is observed that the vitamin K3 level, considering the margin of error, remains largely above 1.5 mg / kg. The amount of vitamin K3 at T+7 months is similar to the amount of vitamin K3 at T+18 months. Conclusion This example shows that a milk powder obtained according to the process of the present invention retains a vitamin K3 content greater than 1.5 mg / kg, or even 2.5 mg / kg (see Table 2: data results at T+7; T+9: T+12; T+18) in the finished product for at least 18 months after its manufacture.

Claims

Process for obtaining a milk powder for young animals enriched with vitamin K3, characterized in that it comprises the following steps: (I) Subjecting the preparation tank, containing the ingredients for producing an animal milk and vitamin K3, to a heat treatment between 20 and 80°C to obtain a mixture, vitamin K3 being added last; (II) Pasteurization of the mixture at a temperature between 70°C and 75°C; (III) Drying of the mixture obtained in step (II) during which a lecithin treatment by spraying soy lecithin simultaneously with the spraying of the milk preparation in the tower is applied to said mixture; (IV) Collection of a milk powder enriched with vitamin K3 at the end of step (III); wherein said vitamin K3 is in the form of menadione nicotinamide bisulfite. Method according to claim 1, wherein the amount of vitamin K3 present in step (I) is between 4 mg / Kg and 6 mg / kg of milk powder. A method according to claim 1 or 2, wherein the heat treatment of step (I) is carried out at a temperature between 40°C and 60°C. Process according to one of the preceding claims, in which the drying step (III) is carried out at inlet temperatures of between 235°C and 245°C and outlet temperatures of between 75°C and 85°C. Milk powder suitable for feeding puppies and kittens, obtained according to the process as defined in one of claims 1 to 3, characterized by a vitamin K3 content greater than 1.5 mg / kg for at least 18 months after production. Milk powder according to claim 4, characterized by a vitamin K3 content of between 1.5 and 10 mg / kg for at least 18 months after production. Milk powder according to claim 4, characterized by a vitamin K3 content of between 2.5 and 10 mg / kg for at least 18 months after production.

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