METHOD FOR OBTAINING A POWDERED MILK FOR PUPPIES AND KITTENS ENRICHED WITH VITAMIN K3
A process for manufacturing vitamin K3-enriched milk powder for puppies and kittens stabilizes the vitamin K3 content by heat treatment, pasteurization, and lecithination, ensuring a stable high content for at least 18 months, overcoming the instability challenges of vitamin K3 in existing formulations.
Patent Information
- Application Number
- FR2023008846
- Authority / Receiving Office
- FR · FR
- Patent Type
- Patents
- Current Assignee / Owner
- Filing Date
- 2023-08-22
- Publication Date
- 2026-10-30
- Estimated Expiration
- 2043-08-22
AI Technical Summary
Existing nutritional compositions for young animals like puppies and kittens lack a stable high content of vitamin K3 due to its instability, particularly sensitive to light, heat, and interactions with choline, leading to significant degradation over time.
A process involving heat treatment, pasteurization, and lecithination of a mixture containing vitamin K3 in the MNB form, followed by drying, to produce a milk powder with a high and stable vitamin K3 content exceeding 1.5 mg/kg for at least 18 months.
The process ensures a high and stable vitamin K3 content in the milk powder, maintaining at least 1.5 mg/kg for 18 months, addressing the instability issues and providing a nutritional product suitable for young animals.
Abstract
Description
Title of the invention: METHOD FOR OBTAINING POWDERED MILK FOR PUPPIES AND KITTENS ENRICHED WITH VITAMIN K3
[0001] The invention relates to the field of high-vitamin nutritional compositions for young animals, such as milk for puppies and kittens. More particularly, the invention relates to a process for obtaining a powdered milk-type nutritional composition characterized by a high vitamin K3 content, this vitamin K3 being in the MNB form. Scope of the invention
[0002] In animal nutrition, it is advantageous to have formulations with high nutritional value. In particular, young animals such as kittens and puppies often require vitamin supplementation. This supplementation is typically provided through the diet, thus supplying all the vitamins and minerals necessary for the animal's health in a simple and inexpensive way.
[0003] Vitamin K3, or menadione, is a synthetic precursor of active vitamin K (biochemically converted into active vitamin K in the body). This vitamin plays an important role in the health of pets, notably enabling blood clotting.
[0004] Vitamin K3, which is generally added to the 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 yield milk with a high vitamin K3 content.
[0005] Vitamin compositions for animals containing vitamin K3 are known from the prior art.
[0006] Document EP1265496 describes a liquid vitamin composition comprising (a) a first liquid vitamin preparation containing 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.
[0007] Document CN112753864 describes a liquid vitamin compound belonging 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.
[0008] The production of vitamin K3 derivatives is also known from the prior art. Document EP2461699 describes vitamin K3 derivative 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 derivative particles (MNB form).
[0009] The prior art also includes sprayable vitamin compositions. Documents CN101874571 and CN101874572 describe vitamin compositions sprayed onto the surface of cat or dog food and the spraying process. The vitamin composition also includes vitamin K3. The spraying process comprises the following main steps: preparation of a base material and the vitamin composition, then spraying the vitamin composition onto the surface of the base material by back-blowing, and finally cooling and packaging to obtain the finished product.
[0010] Due to the instability of this vitamin, there are currently no nutritional compositions available for feeding puppies and kittens that include a high content of vitamin K3 which remains stable, particularly a few months after production. Description of the invention
[0011] The inventors have developed a process for manufacturing a nutritional composition with a high vitamin K3 content in the form of a milk powder, intended for feeding and maintaining the vitamin intake of young animals. The process includes parameters that have been tested and adjusted to guarantee a specific quantity of vitamin K3 in the product obtained for at least 24 months.
[0012] 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 an amount 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 milk powder for young animals enriched with vitamin K3, characterized in that it comprises the following steps:
[0013] (I) Submit the preparation tank, containing the ingredients suitable for production of animal milk and vitamin K3, to a heat treatment between 20 and 80°C to obtain a mixture;
[0014] (II) Pasteurization of the mixture obtained in step (I) at a temperature between 70°C and 75°C;
[0015] (III) Drying of the mixture obtained in step (II) during which a lecithination treatment is applied to said mixture;
[0016] (IV) Collection of a milk powder enriched with vitamin K3 at the end of step (III);
[0017] wherein said vitamin K3 is in MNB form.
[0018] A second object of the invention relates to a milk powder adapted to the feed for 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
[0019] The present invention addresses an unmet need for a milk powder rich in vitamin K3, specifically with a quantity greater than or equal to 1.5 mg / kg of vitamin K3 for at least 18 months after production of said powder, and a nutritional composition suitable for young animals, such as puppies and kittens. The process according to the invention makes it possible to obtain a nutritional product that can be offered in pet stores and by veterinarians. In contrast, vitamin K3-enriched animal milks available on the market state a quantity of vitamin K3 at the time of formulation, but no guarantee is provided regarding how this quantity will change over time. However, it is known that vitamin K3 is the most unstable type of vitamin.
[0020] Vitamin K3 is available in two forms: menadione sodium bisulfite (MSB) and menadione nicotinamide bisulfite (MNB). Of these two forms, vitamin K3 MNB is more resistant and stable than vitamin MSB. However, vitamin K3 MNB is neither water-soluble nor fat-soluble, which poses formulation challenges.
[0021] 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, and on the other hand, the resistant form is not water-soluble. Furthermore, this vitamin is sensitive to light and heat and is also affected by interactions with choline. The amount of vitamin K3 therefore tends to decrease naturally over time. For all these reasons, adding and maintaining a high amount of vitamin K3 in a product formulation poses formulation problems.
[0022] The inventors have developed a process for obtaining milk powder optimized to limit the degradation of vitamin K3 by enriching this milk powder with vitamin K3 in the form of MNB. As a result, it is possible, using the process of the present invention, to formulate compositions with a high vitamin K3 content that remains stable for at least 24 months. This ensures a high vitamin K3 content throughout the shelf life of the milk powder, which is at least 18 months at room temperature (between 15 and 25°C). DETAILED DESCRIPTION OF THE INVENTION
[0023] A first object of the invention relates to a process for obtaining milk powder for young animals enriched with vitamin K3, characterized in that it comprises the following steps:
[0024] (I) Submit the preparation tank, containing the ingredients suitable for preparation of animal milk and vitamin K3, to a heat treatment between 20 and 80°C to obtain a mixture;
[0025] (II) Pasteurization of the mixture at a temperature between 70°C and 75°C;
[0026] (III) Drying of the mixture obtained in step (II) during which a lecithination treatment is applied to the mixture;
[0027] (IV) Collection of a milk powder enriched with vitamin K3 at the end of step (III);
[0028] wherein said vitamin K3 is in MNB form.
[0029] In a preferred embodiment, the amount of vitamin K3 present at step (I) is at least 4 mg / Kg of milk powder.
[0030] By "milk powder" is meant a product obtained from dairy ingredients in powdered form.
[0031] By "ingredients suitable for making animal milk" is meant any ingredient that can be used to formulate milk intended for animals. The ingredients for obtaining a mixture as considered in the invention may include, but are not limited to: a milk preparation containing, for example, milk proteins, fats, fibers, vitamins and minerals, amino acids, choline.
[0032] By "Vitamin K3" is meant any form of vitamin K3, such as, for example, menadione sodium bisulfite (MSB) or menadione nicotinamide bisulfite (MNB).
[0033] By "Vitamin K3 MNB", we mean menadione nicotinamide bisulfite or "Vitamin K3 Menadione Nicotinamide Bisulfite".
[0034] The ingredients constituting the formulation are added directly to the preparation tank in step (I). Vitamin K3 is the last ingredient added. The pH of the mixture in the preparation tank is neutral and its temperature is slightly higher than ambient temperature. The tank is agitated during the processing of the various ingredients at a speed of 400 to 500 rpm. The preparation can be stored in the tank at a temperature between 20 and 80°C for up to 1 hour, with a maximum of 2 hours after the addition of vitamin K3 and before the pasteurization step.
[0035] The inventors have determined that adding vitamin K3 to the process before the drying step avoids the problems typically encountered when formulating vitamin K3.
[0036] 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.
[0037] Step (II) of pasteurization can be carried out at a temperature between 70°C and 75°C. This step will not be described in further detail, as those skilled in the art possess the knowledge required to carry out pasteurization.
[0038] Step (III) of drying the mixture can be carried out by any drying method conventionally used to obtain milk powder. For example, this could be freeze-drying, fluidized bed drying, or hot air drying. The drying according to the invention can be carried out by multi-stage MSD tower spraying with dry air atomization. The drying process includes lecithinization 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.
[0039] In a particular embodiment, the drying step (III) is carried out at inlet temperatures between 235 and 245°C and outlet temperatures between 75 and 85°C.
[0040] 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 ambient temperature.
[0041] 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, and 18 months, for example. The quantity of vitamin K3 present can be determined by chemical analysis using gas chromatography coupled with mass spectrometry (GC / MS).
[0042] In one 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 other 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 quantity of which is stable for at least 18 months, preferably 24 months after the production of said powder. Preferably, the vitamin K3 present in milk powder is in MNB form (this characteristic combines with the ranges of values described above). EXAMPLES
[0043] EXAMPLE 1: Process for obtaining milk powder according to the invention Materials and methods Vitamin K3
[0044] The vitamin K3 used is the bisulfite form of menadione nicotinamide (MNB).
[0045] Fine micro-granular powder, white to yellowish, free-flowing, with complex characteristics. CAS number: 73581-79-0 Empirical formula: Ci7H 16 N2O65 > Molecular weight: 376.39 g / mol Vitamin K3 preparation
[0046] Vitamin K3 is weighed and stored in a pillbox and in an aluminum bag protected from light before production. Preparation of the milk matrix
[0047] Dairy recipe composed of milk proteins, fats, fibers, vitamins and minerals, amino acids, choline.
[0048] Sequence of steps in the preparation of the dairy preparation:
[0049] - Preparation of a dairy base
[0050] - Addition of fats with antioxidants
[0051] - Addition of the premix of vitamins, minerals, fibers and amino acids including choline
[0052] - Addition of vitamin C
[0053] - Addition of vitamin K3
[0054] The pH of the recipe is between 6.7 and 7.0 at 40°C and is stored between 40-55°C before pasteurization. The tank is agitated during the processing of the various ingredients at between 420 and 460 rpm. The preparation is stored in the tank for a maximum of 2 hours after the addition of vitamin K3 and before pasteurization. pasteurization stage
[0055] The product undergoes heat treatment before being sprayed in the drying tower. Pasteurization of the product takes place between 71.8°C and 72.2°C. Drying stage
[0056] Drying is carried out in a multi-stage MSD tower with dry air spraying. The soy lecithin is sprayed simultaneously with the milk preparation in the tower. Conservation
[0057] The powder is packaged in large capacity non-gassed bags in a storage area at ambient temperature. Analytical interpretation
[0058] Vitamin K3 analyses were carried out in several laboratories depending on the progress of the project and the limit of quantification (LOQ). 1. UPSCIENCE: LOQ 0.3 ppm = (A) 2. EUROFINS: LOQ 1 ppm = (B) 3. MERIEUX: LOQ 0.3 ppm = (C) Results
[0059] Pilot tests and then industrial tests were carried out before moving on to production. • Pilot tests
[0060] The tests on the pilot made it possible to validate the approach and to determine the optimal value ranges for the implementation of the process. • Industrial testing
[0061] Industrial-scale trials have provided a better understanding of vitamin K3 losses during the process and have allowed for the determination of the necessary raw material dosage. The results obtained are satisfactory, particularly with an initial vitamin K3 content of 6 mg / kg of milk powder. The average loss is 70.35%. This loss is mitigated by the dilution of the vitamin K3-containing product with the non-vitamin K3-containing product, as the addition is not carried out on complete production runs.
[0062] This dosage allows the vitamin K3 to be found in sufficient quantity with respect to the target defined in the finished product. • Productions
[0063] [Tables 1] Production date Big bag number Average results Vitamin K3 (mg / kg) N'i 2.53 N'2 4.53 N'3 2.53 N'4 2.59 N'5 2.92
[0064] Table 1: Analytical results for vitamin K3 of the productions
[0065] All the results concerning vitamin K3 are consistent and homogeneous. We have an average loss of 54.72% in the process. The loss is lower than in industrial trials because the addition of vitamin K3 was carried out on complete production runs, without dilution. Conclusion
[0066] Following the various tests on the addition of vitamin K3, all the parameters of the process as well as the formulations allowing to obtain in the expected quantity in the finished product were able to be established.
[0067] This example shows that it is possible to obtain a 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.
Claims
Demands
1. A 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 suitable for making animal milk and vitamin K3, vitamin K3 being the last ingredient added, to heat treatment between 20 and 80°C at a pH between 6.7 and 7.0 and with agitation of the tank during the treatment of the different ingredients at between 400 and 500 rpm 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 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.
2. A method according to claim 1, wherein the heat treatment of step (I) is carried out at a temperature between 40°C and 60°C.
3. A process according to claim 1 or 2, wherein the mixture from step (I) is stored in a tank, at a temperature between 20-80°C for a maximum of 2h00 after the addition of vitamin K3 and before the pasteurization step.
4. A method according to any one of the preceding claims, wherein the drying step (III) is carried out at inlet temperatures between 235°C and 245°C and outlet temperatures between 75°C and 85°C.
5. Milk powder suitable for feeding puppies and kittens, obtained according to the process as defined in any one of claims 1 to 4, characterized by a vitamin K3 content greater than 1.5 mg / kg quantified by chemical analysis by gas chromatography coupled with mass spectrometry (GC / MS), for at least 18 months after production.
6. Milk powder according to claim 5, characterized by a vitamin K3 content of between 1.5 and 10 mg / kg as determined by chemical analysis by gas chromatography coupled with mass spectrometry (GC / MS), for at least 18 months after production.
7. Milk powder according to claim 5, characterized by a vitamin K3 content of between 2.5 and 10 mg / kg as determined by chemical analysis by gas chromatography coupled with mass spectrometry (GC / MS), for at least 18 months after production.
