Raw material for animal nutrition comprising an organo-mineral complex containing dietary phosphate and a humic substance
The integration of a humic substance with food phosphate in an organ-mineral complex within animal feed enhances phosphorus bioavailability, addressing digestibility and environmental concerns, and improving overall animal performance.
Patent Information
- Application Number
- FR2020011320
- Authority / Receiving Office
- FR · FR
- Patent Type
- Patents
- Current Assignee / Owner
- Filing Date
- 2020-11-04
- Publication Date
- 2025-03-28
- Estimated Expiration
- 2040-11-04
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Abstract
Description
Title of the invention: Raw material for animal nutrition comprising an organo-mineral complex containing food-grade phosphate and a humic substance. Technical field
[0001] The invention relates to a new phosphate-containing raw material for animal feed. This new raw material combines food-grade phosphate with an organic compound in the form of an organo-mineral complex, which increases the digestibility of inorganic phosphorus in livestock rations and has beneficial effects on certain biological effectors. EARLIER ART
[0002] Phosphorus (P) is a chemical element essential to life on Earth. It plays a vital role in the proper functioning of the metabolism of numerous organisms, both fauna and flora, such as humans, animals, microorganisms, and plants, by participating in energy processes (production of adenosine triphosphate, ATP), bone and tooth synthesis, the composition of deoxyribonucleic acid (DNA) and ribonucleic acid (RNA), the composition of cell membranes (phospholipids, etc.), and the regulation of blood acidity. In fact, global use of mineral phosphates, a source of P, has increased fifteenfold since 1950, and demand is expected to increase by 50 to 100% by 2050 due to global population growth. However, the sources of mineral P (phosphate rock) are not renewable and their stock is destined to disappear in the long term.It is therefore necessary to find alternative solutions or at least to increase the efficiency of the natural phosphate used.
[0003] Phosphorus is therefore an essential element for the good health of animals and the productivity of livestock. It is necessary to add mineral phosphorus to the feed ration of livestock in order to improve weight gain, milk production, bone mineralization, and fertility.
[0004] Regarding animal nutrition, in poultry and pigs a holistic approach is often preferred, in which the requirement is defined as the intake necessary to maximize performance and / or bone mineralization. However, in the case of monogastric animals, improving the digestibility of phosphorus in the ration can be achieved by using more digestible mineral phosphorus sources or by making phytic phosphorus (phytates) in the ration available. Indeed, monogastric animals do not produce phytase, the enzyme Necessary for the hydrolysis of phytates, this form of phosphorus, which is predominant in cereals and oilseed cakes, is very poorly digested by these animals, as it is by humans. This requires utilizing the natural phytases contained in certain cereals and by-products of their processing for human consumption, and especially incorporating phytases of microbial origin into animal feed, which is now a common practice in animal nutrition.
[0005] Unlike monogastric animals, it has long been accepted that little can be expected from the use of microbial phytase in ruminants, as rumen bacteria produce it naturally. Phosphorus (P) is one of the essential minerals for ruminants and is involved in numerous metabolic processes. Rumen bacteria have P requirements 2.0 to 2.5 times greater than the animal's maintenance requirement. This requirement is partially met by dietary intake, but the supply from salivary recycling provides a highly bioavailable form of P, the use of which is favored by rumen microorganisms. P plays an essential role for bacteria, particularly for their structure and ATP synthesis.
[0006] Despite the importance of phosphorus in the rumen (salivary source), it is absorbed by the animal in the duodenum, jejunum, and large intestine. In the diet of a dairy herd, phosphorus will be used for bone growth, energy metabolism, and milk production.
[0007] A deficiency in dietary phosphorus (P) can disrupt milk production, feed intake, and animal performance, leading to a state of latent acidosis that, despite dietary intake, remains unresolved until salivation is sufficient. The solubility of the source is not a determining factor in managing this disorder. In the case of a deficiency, the ruminant system will draw on its P reserves, namely the P stored in tissues or bones. This type of short-term deficiency at the beginning of lactation is not a problem if it is corrected quickly before the start of the second phase of lactation, as is the case with calcium (Ca) metabolism.
[0008] More specifically, the nutritional requirements of a lactating animal are significant during the second phase of lactation because this is when the animal replenishes its reserves. Phosphorus (P) absorption shows little interaction with other minerals, but the calcium (Ca / P) ratio is important. A normal ratio is between 1 and 8 (and up to 16), but an excess of calcium (Ca) can exacerbate the effects of phosphorus deficiency.
[0009] Conversely, if the intake is excessive relative to the requirement, the P will eventually end up in the manure. Research has therefore been carried out to determine more precisely the P requirements, with the aim of ensuring the health and productivity of cows, while minimizing the excretion of this nutrient in the excretion. Excess P is excreted via feces or urine when salivary recycling is saturated, which corresponds to a blood concentration of 2.5-3 mmol / L.
[0010] Based on knowledge of the digestive and metabolic utilization of phosphorus (P), it is possible to determine the P balance in different livestock species, namely the amounts consumed, digested, absorbed, excreted, or deposited in tissues. However, the levels of phosphorus retention efficiency, relative to intake, vary considerably between species. The highest efficiency is obtained in standard chickens (62%), followed by pigs, free-range chickens, and dairy cows (41%, 38%, and 29%, respectively), with laying hens and suckler cows exhibiting the lowest values (21% and 15%, respectively).
[0011] During digestion, the rise in pH in the digestive tract of monogastric animals leads to the recomplexation of ionized molecules of opposite charge initially solubilized in the stomach. These molecular recomplexations, particularly between calcium and phosphate ions, decrease the absorption of the latter in the body. This recomplexation phenomenon therefore results in a decrease in the digestibility of nutrients, and in particular that of minerals. Furthermore, the release into the environment of inorganic phosphorus that has not been absorbed by the animals represents an economic loss for farmers and could soon be limited in accordance with environmental regulations.
[0012] Therefore, it is necessary to improve the bioavailability of inorganic P supplied in the animals' diet.
[0013] It is also detrimental to the quality of digestion to overdose on calcium. In order to limit the negative effects mentioned above in the digestive tract and on the health of animals, it is therefore essential to limit its dose in feed.
[0014] Furthermore, calcium has an inhibitory effect on phytase activity. Manufacturers of monogastric feed therefore tend to overdose phytases to obtain better overall digestibility of the ration and thus maximize zootechnical performance.
[0015] The raw material of the invention contains a food-grade phosphate and a humic substance, such as humic acid, fulvic acid or humates.
[0016] Humic substances are commonly used to improve feed digestibility. The prior art has already described feed or feed raw materials containing humic substances and calcium phosphate, such as patent application CN109198275, which proposes a raw material to improve the nutritional balance of carp and promote their growth. However, in this raw material, the calcium phosphate is not complexed with the humic substance, insofar as they have not been allowed to react. The two compounds are simply mixed dry and ground, so that the complex cannot not to form. Dissolving the humic substance in aqueous solution is necessary to induce complexation. Furthermore, patent application CN109198275 does not address the issue of phosphorus bioavailability in animals.
[0017] The need therefore remains to improve the zootechnical performance of livestock by increasing in particular the digestibility of inorganic phosphorus present in the ration. GENERAL DESCRIPTION OF THE INVENTION
[0018] The invention solves these problems and meets these needs by proposing a feed raw material for animal nutrition comprising an organo-mineral complex containing food phosphate and a humic substance, said humic substance engaging chemical bonds with atoms, such as for example calcium atoms, and / or with the phosphorus atoms of the food phosphate.
[0019] The inventors have indeed found, surprisingly, that the humate-phosphate complex improves the effects of phosphate compared to the results obtained when phosphate is used alone. These effects relate in particular to zootechnical performance, phosphorus digestibility in the ration, and the regulation of certain biological effectors.
[0020] The inventors have indeed shown that the nutritional properties of phosphorus of mineral origin can be improved by complexing it with a humic substance.
[0021] The processes of administering humic substances and phosphate separately, as described in the prior art, as food raw materials and adding them dry to the ration without having previously reacted them with each other, do not allow these effects to be obtained.
[0022] Without being bound by any theory, the inventors believe that, in the case of calcium phosphate, the complexation of calcium with the humic substance renders it at least partially unavailable in the digestive tract and thus increases both the efficiency of phosphorus digestion and the activity of phytases. The raw material of the invention therefore makes it possible to reduce the required dose of phosphate and / or the required dose of phytases in food.
[0023] The present invention arises from the surprising advantages demonstrated by the inventors of the effect of complexation of calcium and / or phosphate ions by humic substances on the bioavailability of phosphorus during digestion in a monogastric animal. The digestibility of inorganic phosphorus is indeed improved by using a complex between mineral phosphorus and an organic molecule based on a humic substance, particularly humates or humic acids. This results in, among other things, improved digestibility of the ration (and of phosphorus in particular). For all species, this results in improved bone mineralization (for chickens and hens, for example, which reduces lameness in poultry farming and delays culling of laying hens) and better eggshell quality (for hens), which reduces egg downgrading rates and increases hatching rates and chick viability. Beyond these nutritional benefits, the raw material of the invention also offers advantages for farmers, as it allows for ingredient savings and increased productivity. Binding calcium with a humic substance limits many reactions of this cation with other elements present in the digestive tract. These reactions are often a source of performance losses. The raw material of the invention therefore leads to improved feed efficiency and thus reduces phosphorus emissions into the environment.
[0024] More specifically, the organo-mineral complex allows for the maintenance of zootechnical performance if it is incorporated at a dose that allows reaching 80% of the usual phosphorus requirements.
[0025] The raw material of the invention also makes it possible to fight against mycotoxins because it is capable of adsorbing them at different pH levels during digestion.
[0026] More specifically, in the digestive tract, the organo-mineral complex is able to adsorb some of the aflatoxins and other mycotoxins initially present in the ration. DETAILED DESCRIPTION OF THE INVENTION
[0027] The raw material for animal nutrition comprising an organo-mineral complex containing food phosphate and a humic substance, said humic substance engaging chemical bonds with phosphorus atoms.
[0028] Dietary phosphate can be anhydrous or hydrated. Dietary phosphate can be selected from calcium phosphate, magnesium phosphate, monosodium phosphate (MSP), calcium-sodium phosphate, and mixtures thereof. In the raw material of the invention, the dietary phosphate can be selected from monocalcium phosphate (MCP), dicalcium phosphate (DCP), monobicalcium phosphate (MDCP), tricalcium phosphate (TCP), and mixtures thereof. The phosphate can also be in the form of trimagnesium phosphate.
[0029] In a particular embodiment, the food phosphate contains or is made up of calcium phosphate.
[0030] When the food-grade phosphate is, for example, calcium phosphate, the humic substance forms chemical bonds between the molecules it contains and the calcium and / or phosphorus atoms contained in the calcium phosphate. This raw material can be obtained from a calcium source, a phosphorus source, and a humic substance and is present in the form of dietary phosphate. When dietary phosphate is sodium phosphate, calcium sodium phosphate or magnesium phosphate, the humic substance can engage in chemical bonds between the molecules it contains and the sodium atoms and magnesium atoms respectively.
[0031] In this case, the raw material comprises a humic substance that is complexed with calcium and / or phosphorus. The raw material of the invention may contain, in addition to calcium phosphate, magnesium phosphate, sodium phosphate, and / or a mixed sodium and calcium phosphate.
[0032] In the particular embodiment of the invention in which the dietary phosphate contains calcium phosphate, the humic substance acts first by complexing with the calcium cations. The advantage of this complexation is, in particular, to increase the bioavailability of phosphorus by rendering the calcium unavailable. The humic substance then plays a role in the metabolic reactions taking place in the digestive tract by remaining at least partially complexed with calcium after passing through the stomach. The free fraction of the humic substance can spontaneously complex with other cations present in the digestive tract, particularly ionized free calcium.
[0033] For the purposes of this invention, "humic substance" means a molecule or set of molecules of natural origin conforming to the definition of the International Humic Substance Society (IHSS), according to which humic substances are complex and heterogeneous mixtures of polydisperse materials formed in soils, sediments, and natural waters by biochemical and chemical reactions during a process of decomposition and transformation of plant and microbial remains, a process known as humification. Many compounds participate in humification, such as plant lignin and its transformation products, polysaccharides, melanin, cutin, proteins, lipids, nucleic acids, and carbonization residues.
[0034] The main molecules present in humic substances include dark brown or grey-black humic acids (HA), light yellow or yellow-brown fulvic acids (FA), and black humin. The darker the color of the humic substance, the higher the molecular weight of the molecules it contains, the higher the carbon content, the lower the oxygen content, and the lower the acidity exchange.
[0035] According to one embodiment of the invention, the humic substance is chosen from among sodium-based humates, having a higher ion exchange capacity, the sodium ion being more easily exchanged in the digestive tract of the animal compared with a divalent calcium or potassium ion.
[0036] The humic substance can be prepared by treating naturally occurring humic substances in acidic form with an appropriate amount of a strong base, such as sodium hydroxide or potassium hydroxide, to obtain soluble humic substances with a carboxylate functional group, which will be referred to as humates in this description. For example, the starting material in the form of humic acids naturally present in soil can be used to produce humates. The humates can be obtained in the form of an aqueous solution or in dry form, which can then be dissolved in water.
[0037] Depending on the humic substance content in the raw material, the amount of calcium and the amount of complexed phosphorus varies.
[0038] Thus, this complexation can be demonstrated by any method known to those skilled in the art, in particular by X-ray diffraction (XRD) or phosphorus-31 nuclear magnetic resonance (P31NMR). The presence of calcium or phosphorus complexed by humates, as well as the presence of some free cations and anions, in the product of the invention, can be imagined. The exact percentage of complexed ions, particularly calcium and phosphorus, could not be measured.
[0039] An aqueous dispersion of humic substances may contain a significant amount of insoluble matter. This is the case, for example, when the liquid composition of humic substances is prepared from raw material mixed with water. In this particular case, the soluble fraction can be isolated by separating it from the insoluble fraction, for example by decantation, filtration, or centrifugation.
[0040] The humic substance can be obtained from natural humic substances. For example, it can be a raw material containing humic substances, such as peat, leonardite, lignite, coal, or anthracite. Thus, the humic substance can be a liquid composition of peat, leonardite, lignite, coal, or anthracite. In a particular embodiment of the invention, the humic substance is extracted from leonardite.
[0041] Peat is a fossil organic material formed by the accumulation, over long periods of time, of dead organic matter, primarily plants, in a water-saturated environment. Peat makes up the majority of peatland soils. Peat can be more or less rich in humic substances depending on the degree of decomposition. The degree of decomposition of peat is classified according to the Von Post scale, which ranges from H1 (least decomposed peat) to H10 (most decomposed peat). Humus peat, that is, peat classified from H6 to H10 according to the Von Post scale, is the preferred peat for implementing the process according to the invention because it is richer in humic substances than peat classified from H1 to H5 according to the Von Post scale.
[0042] Leonardite is a rock that can contain more than 90% by weight of humic substances. This rock has undergone more degradation than peat, but less than coal.
[0043] Lignite is a sedimentary rock composed of fossilized plant remains. It is an intermediate rock between peat and coal.
[0044] Coal is a sedimentary carbonaceous rock corresponding to a specific quality of coal, intermediate between lignite and anthracite. Blackish in color, it originates from the carbonization of plant organisms.
[0045] Anthracite is a sedimentary rock of organic origin. It is a grey, blackish and shiny variety of coal extracted from mines.
[0046] Humic substances can also be obtained from synthetic humic substances. Synthetic humic substances can, for example, result from a synthesis process or from the transformation of natural humic substances, in particular by semisynthesis.
[0047] The humic substance can also be extracted from organic materials (peat, leonardite, lignite, coal, anthracite, soils rich in humic substances, composts of plant waste, etc.) using an alkaline agent such as sodium hydroxide (NaOH) or potassium hydroxide (KOH) and optionally subjected to purification. Humic substances can, in particular, be extracted and / or purified by processes well known to those skilled in the art. The humic substance can be a potassium humate or, preferably, a sodium humate.
[0048] Humic substances encompass liquid compositions of a salt of humic substances. Preferred salts include ammonium salts, sodium salts, and potassium salts. Preferably, a sodium salt of humic substances, such as sodium humate or sodium salt of humic substances, is used due to its high ion exchange capacity. Salts of humic substances are commercially available. For example, potassium salt of humic substances is marketed by Humatex under the brand name Dralig® (CAS 68514-28-3). The Dralig® product is prepared from humic substances extracted from Czech natural oxyhumolite with a high humic substance content. Sodium humate (CAS number 68131-04-4), commercially available under the brand name Nut Mordan®, manufactured by Humatex, is another example. A person skilled in the art will have no difficulty in preparing a salt from humic substances.
[0049] The purity of the humic substance in humic molecules can also vary, for example depending on the source used. Of course, peat is generally less pure in humic substances than leonardite or a commercial powder. of humic substances. In a particular embodiment, the humic substance comprises at least 50% by dry mass of humic molecules.
[0050] The invention also relates to a method for manufacturing the food raw material described above, said method comprising a step of preparing an aqueous dispersion or an aqueous solution containing the humic substance, followed by mixing this dispersion or this solution with a source of phosphorus and with a source of calcium, magnesium or sodium.
[0051] The complexation of the humic substance with phosphorus atoms, and optionally with calcium, magnesium, or sodium atoms, and the formation of chemical bonds between the humic substance and the phosphorus atoms can be achieved by the presence of the humic substance in a reaction mixture containing the phosphorus source and the calcium, magnesium, or sodium source. The chemical bonds can be formed by the insertion of the humic substance during the reaction between the phosphorus source and the calcium, magnesium, or sodium source. In a particular embodiment, the chemical bonds of the organo-mineral complex are formed by the insertion of humates during the reaction between the phosphorus source and the calcium source.
[0052] The food raw material described above can be obtained by preparing an aqueous dispersion or aqueous solution containing the humic substance, the phosphorus source, and the calcium, magnesium, or sodium source. For example, the food raw material of the invention is obtained by preparing an aqueous dispersion or aqueous solution containing the humic substance, followed by mixing this dispersion or solution with the phosphorus source and with the calcium, magnesium, or sodium source.
[0053] The mixing of the aqueous dispersion or aqueous solution containing the humic substance with the phosphorus source and the calcium, magnesium or sodium source can be carried out at a temperature ranging from 50°C to 80°C, preferably from 60°C to 80°C.
[0054] A process for manufacturing the food raw material may include a step of purifying a humic substance to obtain humates which can then be solubilized in water.
[0055] The calcium source that can be used to prepare the raw material of the invention can be calcium carbonate (CaCO3), quicklime (CaO), or even slaked lime (Ca(OH)2). The phosphorus source can be phosphoric acid. The calcium, magnesium, or sodium source, and the phosphoric acid react with the humic substance placed in solution or aqueous dispersion.
[0056] The raw material of the present invention can be manufactured by various methods depending on how the humic substance is mixed at the source of calcium, magnesium or sodium, and to the phosphorus source. For example, the humic substance can be introduced simultaneously but separately from the other raw materials, introduced in a premix with the calcium, magnesium or sodium source, mixed with the phosphorus source before dissolving in water, introduced into the phosphorus source once dissolved in water, or introduced into the water.
[0057] According to a particular embodiment, the humic substance is a humate mixture that is dissolved in water to obtain an aqueous humate solution, which solution is then mixed with phosphoric acid while stirring. The resulting dispersion may be mixed with calcium carbonate. The P₂O₅ content of the phosphoric acid may range from 52% to 60%. The humate concentration in the aqueous humate solution may range from 50 g / L to 250 g / L of water. In the aqueous dispersion containing the humates and phosphoric acid, the phosphoric acid is preferably diluted to between 40% and 55% P₂O₅.
[0058] The humic substance represents, for example, between 0.1% by mass and 10% by mass of the mass of a mixture consisting of i) a source of calcium, magnesium, or sodium, ii) the source of phosphorus, and iii) the humic substance. When the humic substance is humate-based, the dose of humates in the raw material of the invention may be between 1.0% and 10.0%, preferably between 1.0% and 5.0%, more preferably between 1.0% and 3.0% by mass, and even more preferably between 1.0% and 2.5%, for example equal to 1.5% by mass, of the mass of said mixture.
[0059] The process according to the invention may include one or more additional steps, for example one or more granulation or drying steps.
[0060] Another object of the invention relates to the use of a raw material as described above to improve the bioavailability of mineral phosphorus in a monogastric livestock animal. The invention is a means of supplying minerals and inorganic phosphorus, particularly to monogastric animals, but also to ruminants.
[0061] The invention also relates to a method of feeding a farm animal comprising a step of incorporating into the animal's ration the raw material described above, this raw material possibly being produced prior to the process described above.
[0062] The invention further relates to a method for manufacturing a premix or complete feed for livestock. The raw material of the invention is intended for use in premixes or complete feeds for premixers or feed manufacturers for livestock.
[0063] The raw material can be used for poultry (standard or label broiler chickens, laying hens, turkeys, guinea fowl, ducks and others), but also for pigs, cattle, sheep, goats, rabbits, and aquaculture. DESCRIPTION OF THE FIGURES
[0064] [Fig. 1] The [Fig. 1] represents the X-ray diffractogram of a reference product containing humic substance-free monocalcium phosphate (MCPHO).
[0065] [Fig.2] Fig.2 represents the X-ray diffractogram of a product of the invention containing 1.5% humates (MCPH15).
[0066] [Fig.3] Fig.3 compares the two diffractograms of the previous Figures 1 and 2.
[0067] [Fig. 4] Figure 4 shows the 31P NMR spectra of a reference product containing of monocalcium phosphate devoid of humic substance (MCPHO), and that of the product of invention containing 1.5% humates (MCPH15).
[0068] [Fig.5] The [Fig.5] represents the 31P NMR spectrum of a reference product containing humic substance-free monocalcium phosphate (MCPHO).
[0069] [Fig.6] Fig.6 represents the 31P NMR spectrum of the product of the invention containing 1.5% humates (MCPH15).
[0070] [Fig.7] Fig.7 shows the effect of the invention on the evolution of the pH of the ruminai medium from 2.0 to 6.5 hours of incubation under in vitro fermentation conditions.
[0071] [Fig.8] Fig.8 shows the effect of the invention on the concentrations of VFA in the ruminal medium from 2.0 to 6.5 hours of incubation under in vitro fermentation conditions.
[0072] [Fig.9] Fig.9 shows the effect of different doses of the invention on the rate of adsorption of various mycotoxins in the stomach of monogastric animals under in vitro conditions.
[0073] [Fig. 10] Fig. 10 shows the effect of different doses of the invention on the rate of adsorption of various mycotoxins in the intestine of monogastric animals under in vitro conditions.
[0074] [Fig. 11] Fig. 11 presents the average feed conversion ratio (FCR) at the end of finishing (FCR-35 between J0 and J35) of batches of chickens whose feed has been enriched with different MCPs containing or not different doses of humates.
[0075] [Fig. 12] Fig. 12 shows the ash content and the amount of calcium and phosphorus in the tibias of chickens taken at day 35 according to the treatments.
[0076] [Fig. 13] Fig. 13 shows the fracture strength of the tibias of chickens taken at day 35 according to the treatments.
[0077] [Fig. 14] Fig. 14 shows for each treatment the difference (%) in pH of chicken meat between the measured value and the value to be reached after 15 minutes of maturation (pH = 6.4) or 7 days of storage (pH = 5.6).
[0078] [Fig. 15] Fig. 15 shows the average feed conversion ratio (FCR) at the end of finishing (FCR-35 between JO and J35) of batches of chickens whose feed has been enriched with a standard calcium phosphate or the product of invention MCPH15.
[0079] [Fig. 16] Fig. 16 shows the amount of P2O5 in the litter at day 42 of chickens that received in their feed a standard calcium phosphate or the product of invention MCPH15.
[0080] Example 1: Preparation of a humate and calcium phosphate complex followed by characterization
[0081] Preparation of the complex
[0082] Several aqueous solutions of sodium humates with varying humate concentrations ranging from 100 g / L to 250 g / L are prepared by solubilizing sodium humates in water, preferably water heated to 50°C.
[0083] Sodium humate (CAS number 68131-04-4) is commercially available under the brand name Nut Mordan®, manufactured by Humatex. The pH of this product diluted to 10% in water is between 10.0 and 12.0, and its humic acid content by dry weight is greater than 60%. The humic acid content by dry weight is equal to the complement to 100% of the ash content measured after calcination of the sample in an electric furnace at 500°C for 60 minutes and at 805°C–825°C for 60 minutes (according to the manufacturer).
[0084] A solution of Israeli green phosphoric acid (total P2O5=54.2%) diluted to 50% P2O5 with water heated to 50°C is prepared.
[0085] Each aqueous solution of humates is then poured under stirring into the phosphoric acid solution, stirring being maintained to disperse the solid formed and the temperature maintained at 50°C. Calcium carbonate (having a total CaO content greater than or equal to 53%) is then added to the dispersion, and the mixture is then stirred vigorously, clumped, granulated and then dried.
[0086] Alternatively, the phosphoric acid is not diluted in water and is poured simultaneously into the sodium humate solution on the calcium carbonate.
[0087] The mass ratio between undiluted phosphoric acid at 54% P2O5 in water and calcium carbonate was 2.5 for manufacturing MCP.
[0088] By varying the concentration of the humate solution, monocalcium phosphates containing 1.0% (noted MCPH10), 1.5% (noted MCPH15), 2.0% (noted MCPH20), 2.5% (noted MCPH25), 5.0% (noted MCP50) and 10.0% (noted MCP100) of humates could be prepared.
[0089] Dicalcium phosphates containing 0% (denoted DCP), 1.0% (denoted DCP10), 5.0% (denoted DCP50) and 10.0% (denoted DCP100) of humates by applying a mass ratio [phosphoric acid at 54%P2O5 / calcium carbonate] = 1.3. could also be prepared.
[0090] In most of the tests, and in order to limit the number of invention samples studied, the choice was made to doses between 1.0% and 2.5%, preferably 1.5%.
[0091] Characterization by XRD and NMR
[0092] Experimental conditions for XRD analysis:
[0093] The diffractograms were recorded on a diffractometer (PANalytical brand X'Pert Pro) in reflection mode, equipped with a copper tube (Ka = 0.1542 nm, 45 kV and 40 mA) and a PIXcel linear detector (active length = 3.347 °20). The primary optics in the X-ray beam path consisted of 0.04 rad Soller slits, a 1 / 16° divergence slit, a 10 mm mask, and a 1 / 8° anti-scattering slit. The secondary optics consisted of a nickel filter and 0.04 rad Soller slits. After fine grinding, the samples were compacted in a rear-loading sample holder.
[0094] Results of the XRD analysis:
[0095] The diffractogram peaks revealed that the humate-free MCP (MCPH0) consists of two crystalline phases: predominantly monocalcium phosphate monohydrate (Ca(H2PO4)2.H2O) and, to a lesser extent, calcite (calcium carbonate; CaCO3). However, three very weak peaks above 65° could not be identified, as the reflections from the reference map were only recorded up to 64° ([Fig. 1]). This indicates that an additional crystalline phase is present in the MCPH0 but cannot be identified by XRD.
[0096] The diffractogram peaks of MCPH15 reveal that this sample contains mainly monohydrated monocalcium phosphate (Ca(H2PO4)2.H2O), probably anhydrous dicalcium phosphate (monetite Ca(HPO4)), and possibly calcite (calcium carbonate; CaCO3) and anhydrous monocalcium phosphate (Ca(H2PO4)2) ([Fig. 2]). However, the diffractogram of MCPH15 shows less intense diffraction peaks than that of MCPH0, indicating that this sample is less well crystallized.
[0097] To confirm this, when the two diffractograms of the two samples are superimposed, it can be seen that the baseline of sample MCPH15 between 15 and 40° is higher than that of sample MCPH0 ([Fig. 3]). This therefore indicates the presence of amorphous material in sample MCPH15. Furthermore, organic matrices cannot be identified by X-ray diffraction and thus appear as an amorphous phase. This decrease in peak intensity and this higher baseline of MCPH15 are explained by the presence of humates which correspond to a non-crystalline organic product with an amorphous phase not identified by XRD. In general, organo-mineral complexes characterized by XRD show a broadening of the curves which indicates the presence of an amorphous product in the sample.
[0098] Experimental conditions for NMR analysis:
[0099] After fine grinding, the samples (powders) were introduced (tamped) into a 4 mm diameter cylindrical zirconium oxide sample holder (rotor) closed with a Kelefl® stopper. Analyses were performed at room temperature using a Bruker Avance II 400 MHz spectrometer (Larmor frequency (31P) = 103.85 MHz), equipped with a Bruker 4 mm dual-channel measuring head. The 31P MAS (Magic Angle Spinning) spectra were recorded at a rotation speed of 12 kHz with a pulse angle of 3 µs and a recycle time of 200 s. Chemical shifts are expressed relative to an 85% aqueous H3PO4 solution. After analysis, the samples were fully recovered.
[0100] Results of the NMR analysis:
[0101] Figure 4 shows the superposition of the 31P NMR spectra of the two analyzed samples. More specifically, Figure 5 shows that after deconvolution, the spectrum of MCPH0 exhibits four signals at 0.75, -0.15, -1.45, and -4.65 ppm. The signals at -0.15 and -4.65 correspond to the presence of monocalcium phosphate monohydrate (Ca(H2PO4)2·H2O), the major component (80%), as demonstrated by the XRD analysis. Furthermore, these two signals correspond to two distinct H2PO4 groups: the one at -4.65 is a hydrogen bond acceptor with the protons of the water molecule, while the one at -0.15 is a hydrogen bond donor. The two larger signals at -1.45 and 0.75 ppm characterize the crystallographic sites of dicalcium phosphate (CaHPO4) not revealed by XRD and in minor quantity in this sample (20%).
[0102] Figure 6 shows that after deconvolution, the spectrum of MCPH15 exhibits five signals at -0.1, -0.2, -1.75, -4.75, and -10.0 ppm. As in sample MCPH0, the characteristic signals of monocalcium phosphate monohydrate (Ca(H2PO4)2·H2O) are observed at -0.2 and -4.75 ppm, but in a lower proportion (40% of the sample), their corresponding peaks being weaker than for MCPH0. The peak at -1.75 ppm corresponds to the peak at -1.45 ppm of MCPH0, thus indicating the presence of dicalcium phosphate (CaHPO4) at a level of 10%. However, for MCPH15, it is impossible to distinguish the equivalent of the 0.75 ppm peak of MCPH0, which also indicates the presence of this dicalcium phosphate. Thus, the particularly broad signal at -0.1 ppm would correspond to the superposition of several chemical elements, namely: the missing part of monocalcium phosphate monohydrate (Ca(H2PO4)2.H2O; i.e. 20%), the invisible resonance of this dicalcium phosphate (CaHPO4; i.e., 10%), and a hidden portion of anhydrous monocalcium phosphate (Ca(H2PO4); at a level of 5% to 10%), the only phosphate component whose chemical shifts can be found in the range around -0.1 ppm. Although present in very small quantities, this latter compound can only exist in amorphous form, explaining the characteristic shape of the very broad signal. Finally, the very broad signal between -6.0 and -12.0 ppm corresponds to amorphous [3-Ca2P2O7] pyrophosphates, present at approximately 15% in the sample. This amorphous characteristic is highlighted by the signal width, which indicates that the environment of the phosphate is very disordered and therefore altered. This peak reflects the new environment of the phosphate, which could be linked by Ca-humic acid binding sites, highlighting the complexation of humic acids with minerals (Ca or P).The broadening of these two peaks, indicative of amorphous phases, highlights a chemical reaction between phosphorus sources and humates, indicating the presence of complexes.
[0103] Thus, the results of the XRD and 31P NMR analyses of the two samples are consistent and complementary. Regarding sample MCPH0, both methods confirm the presence of monohydrated monocalcium phosphate (Ca(H2PO4)2.H2O). Unlike XRD, 31P NMR reveals the presence of dicalcium phosphate, also known as monetite (CaHPO4), in MCPH0, likely in amorphous form (broad signals at -1.45 and 0.75 ppm of the NMR), as it was not detected by XRD. This means that the three unidentified peaks above 64° do not correspond to this monetite. However, XRD reveals that crystallized calcite (CaCO3) remains in MCPH0. Finally, NMR31P allows us to estimate that the relative proportions of phosphorus are distributed as follows: as the major phase 80% of Ca(H2PO4)2.H2O and approximately 20% of CaHPO4.
[0104] Regarding sample MCPH15, 31P NMR confirms the presence of crystalline phases observed by XRD, namely: monohydrated monocalcium phosphate (Ca(H2PO4)2.H2O), which is the predominant component, followed by monetite (CaHPO4). Anhydrous monocalcium phosphate (Ca(H2PO4)2), amorphous or very poorly crystallized (as it is possibly visible by XRD), is also present. 31P NMR also reveals the presence of a new species, calcium pyrophosphates (|3-Ca2P2O7), which are in amorphous form since they were not identified by XRD. According to XRD, residual traces of calcite also appear to be present. Other types of amorphous phases were also identified. Some of the amorphous phases not fully identified by NMR are linked to the presence of complexes in the sample, highlighting that a chemical reaction has taken place between the phosphorus sources. and humates. We can imagine physico-chemical bonds between the humate-type organic matrix and the minerals present in the system (calcium and phosphorus). Finally, 31P NMR allows us to evaluate the phosphorus distribution in a very relative way as follows: the major phase, more than 50% Ca(H2PO4)2 .H2O, several minor phases (less than 50%) have been identified, including CaHPO4, amorphous pyrophosphates, and partially crystallized Ca(H2PO4)2, as well as an amorphous phase represented by broadenings of the spectra (curves) corresponding to our organo-mineral complex.
[0105] Thus, both XRD and NMR analyses reveal the presence of amorphous phases equivalent to an organo-mineral complex resulting from chemical reactions in the medium between humic acids and inorganic compounds (calcium phosphates).
[0106] Example 2: In vitro test on an artificial fermenter: impact of the product of the invention on fermentation parameters
[0107] An artificial fermenter test was conducted with the four invention products MCPH0, MCPH10, MCPH5 and MCPH100 prepared according to Example 1.
[0108] Experimental protocol
[0109] The principle of artificial fermentation is based on the incubation of rumen juice under anaerobic conditions at 39°C (Menke and Steingass, 1988). The bacterial flora, in the presence of the appropriate substrate, reproduces ruminal fermentations, which allows for monitoring gas production as well as end products such as volatile fatty acids (VFAs), N-NH3, etc., according to the objectives of the study.
[0110] The device consists of 21 vials of 250 ml each containing 150 ml of an inoculum based on rumen fluid and buffered artificial saliva (1:2). This inoculum is incubated under anaerobic conditions at 39°C without substrate (Blank) or with 1.25 g of substrate (corn silage, hay, concentrate: 50 / 30 / 20, providing 2.2 g of P / kg) alone (Control CT) or with the substrate supplemented with the appropriate dose of each product tested to obtain an identical phosphorus intake (MCPH0 to MCPH100). The vial sampling system will allow for kinetic analysis at 2 h, 4 h, and 6.5 h. Table 1 summarizes the experimental design of the trial.
[0111] [Table 1] Experimental design of the in vitro fermentation test in the presence of the products of the invention Product Substrate Concentration P (%) Product dose (g / D / VL) Number of vials CT EM / F / C - - 4 MCPH0 50 / 30 / 20 22.4 100 4 MCPH10 22.5 99.6 4 MCPH5 21.9 102.3 4 MCPH100 21.7 103.2 4 White - - - 1 Total 21
[0112] Results
[0113] Figure 7 shows the pH evolution at the beginning and end of fermentation. Treatments and time have a significant effect (p < 0.001). The high dose (10%) of humic acid in the MCP increases the pH compared to the control and the other treatments. Furthermore, the "treatment*time" interaction is significant (p = 0.06). It therefore appears that the impact of the treatments varies depending on the kinetic points.
[0114] Figure 8 shows that VFA concentrations increase over time (p < 0.001). Certain treatments, in particular, tend to increase total VFA production compared to the CT control (p < 0.10). Statistical analysis of this parameter reveals a significant interaction between treatments and time (p = 0.02). The results of the statistical analysis at each time point show that after 2 hours of fermentation, high doses of humic acids tend to reduce VFA production (p = 0.07). After 4 hours, the treatments have no effect (p > 0.10). Finally, after 6 hours, MCP supplementation increases VFA production, and the formulas with 1% and 10% humic acids promote this effect (p < 0.01).
[0115] Conclusion
[0116] This in vitro study evaluated the effect of the MCP-Humates complex on rumen fermentation. Supplementation with the MCP-Humates complex limited the drop in pH during fermentation under these closed batch conditions. Furthermore, it improved the production of volatile fatty acids (VFAs) and therefore the energy supply for the ruminant.
[0117] Example 3: Monogastric in vitro digestion test: impact of the product of the invention on the digestibility of the minerals Ca, P and Mg
[0118] The purpose of this in vitro digestion test is to evaluate the digestibility of the minerals Ca, P, and Mg in the products of invention of Example 1. To confirm the results, the test was repeated once. The results of the two in vitro tests conducted are presented below: Test 1 and Test 2.
[0119] Experimental protocol
[0120] The device used is a water bath composed of 15 places, each able to accommodate a 50 ml Eppendorf tube, each containing a 1.0 g food sample. The samples are incubated at 40°C. A test is carried out in 3 stages to mimic the digestion of growing chickens, in the crop (amylase, pH: 5.8, duration: 35 min), then the succenturiate ventricle (pepsin, pH: 2.7, duration: 42 min) and finally in the intestine up to the ileal phase (pancreatin, pH: 6.5, duration: 170 min).
[0121] The water bath can hold 15 samples, and a test is conducted over one day to obtain a sufficient number of replicates per feed (n = 3). Of the 15 tubes, one is used to check for the absence of mineral contamination (blank, no sample) and one is used to receive wheat bran (laboratory standard) to verify the proper conduct of the test. Nine tubes are used to receive samples of complete feed for growing chickens containing the products of the invention at the following humate concentrations: 0% and 1.5%.
[0122] The chemical composition of the food put to be digested is given in Table 2.
[0123] [Table 2]. Nutritional composition of the two experimental feeds for growing chickens. % MCPH0 Feed MCPH15 Feed Moisture 17.5 11.0 DM 82.5 89.0 MM 6.0 5.7 MO 94.0 94.3 Protein 18.8 18.8 Ca 0.84 0.78 P 0.49 0.48 Mg 0.17 0.16 Na 0.17 0.16 Ca / P 1.71 1.63 In vitro digestibility is expressed by calculating the solubility of minerals. In other words, the greater the quantity of minerals in the liquid of the food bolus (ileal fluid), the better the potential absorption of these minerals. Solubility is calculated as follows: Solubility (%) = quantity of mineral in ileal fluid / quantity of mineral in 1 g of food to be digested.
[0124] Results An in vitro digestion assay was conducted in which MCPH0 and MCPH15 were compared. The results were as follows.
[0125] The solubility of chicken feed supplied with MCPH0 or MCPH15 manufactured according to Example 1 is given in Table 3.
[0126] [Table 3] Solubility of minerals in the monogastric in vitro digestion test as a function of treatments based on or not on the product of invention (Mean ± SD). I Food fn Solubility Solubility P (%) Solubility Mg (%) I Ca(%) MCPH0 2 59.6 (± 0.74) 68.2 (±3.15) 57.8 (± 2.99) MCPH15 3 62.9 (±0.91) 72.2 (± 0.92) 62.2 (± 0.69) p.val - 0.02 0.11 0.08
[0127] The solubility of calcium is significantly affected by the presence of humates (p = 0.02). Furthermore, the solubility of calcium is significantly higher by 3 percentage points in the presence of 1.5% humates than in their absence. Similarly, the solubility of phosphorus is not significantly higher (p = 0.11) by 4 percentage points in the presence of humates than in their absence. Finally, the solubility of magnesium is also not significantly higher (p = 0.08) by 4 percentage points in the presence of humates than in their absence.
[0128] Conclusion The results showed that the solubilities of calcium (Ca) and phosphorus (P) in the test feed are affected by the presence of humate-rich protein concentrates (PCCs). These results demonstrate that the solubilities of Ca and P are significantly improved in the presence of humates (by 3 and 4 percentage points, respectively). The solubility of magnesium (Mg) is consistently significantly improved (by 1 to 4 percentage points) in the presence of humates, regardless of the digestion trial.
[0129] Example 4: In vitro study of the adsorption capacity of mycotoxins by the product of the invention in the digestive tract of monogastric animals
[0130] The present in vitro study aims to evaluate the mycotoxin adsorption capacity of the product of the invention under monogastric digestive conditions. The principle consists of bringing the product into contact with a given dose of mycotoxins at a given temperature and pH.
[0131] Experimental protocol
[0132] Four mycotoxins were chosen based on the frequency of their presence in feed or plant-based raw materials intended for monogastric animals, as well as the sensitivity of poultry and pigs (young and adult) to them. The dose of each of these four mycotoxins was determined according to European regulations (aflatoxin B1) and the sensitivity of the two species (zearalenone, ochratoxin A, and deoxynivalenol). Thus, three doses (0.5%, 0.8%, and 1.0%) of the product of invention MCPH15 were brought into contact with 100 to 900 ng / ml of mixed mycotoxins (Table 4).
[0133] [Table 4] Doses of mycotoxins and product of invention introduced into the intromonogastric digestive system Mycotoxin Mycotoxin dose (ng / ml) Invention product dose (g / 100g) aflatoxin B1 20 0.5 zearalenone 250 0.8 1.0 ochratoxin A 100 deoxynivalenol 900
[0134] The concentration of mycotoxins was measured after each incubation time to determine the amount adsorbed by the product.
[0135] Mycotoxin concentrations were measured by UHPLC-MS / MS. Specifically, a 0.1 M buffered phosphate solution at pH 2.50 ± 0.05 (average stomach pH between pig and poultry) was prepared and enriched with mycotoxins at the concentrations listed above. The sample was added to the mycotoxin-enriched solutions, and the suspension was then incubated at 40°C for 1 hour. The suspension was then centrifuged, and the supernatant was sampled. The remaining supernatant was discarded, and the test material was then resuspended in a 0.1 M buffered phosphate solution at pH 6.80 ± 0.05 (average intestine pH between pig and poultry) before being incubated at 40°C for a further 3 hours. The suspension was again centrifuged, and the supernatant was sampled. Sample solutions were enriched with isotopically labeled internal standards before being analyzed by UHPLC-MS / MS.Quantification was performed using external calibration solutions enriched with isotopically labeled internal standards. All samples were prepared in quintuplicate.
[0136] The calculation of the adsorption rate is as follows:
[0137] Stomach adsorption rate (%) = (initial [mycotoxin] - stomach supernatant [mycotoxin] ) / [mycotoxin]initiated; Final adsorption rate (%) = l-(([mycotoxin]stomach supernatant + [mycotoxin]intestinal supernatant) / [mycotoxin]initiated).
[0138] Results
[0139] The results show that the higher the dose of product in the system, the higher the adsorption rate. Adsorption rates at low pH (stomach level) are also higher than at high pH (intestinal level). Upon passage into the intestine, the rise in pH results in some desorption of the mycotoxins. More specifically, the adsorption capacity is, in decreasing order: aflatoxin > zearalenone > ochratoxin > deoxynivalenol. Once in the intestine, the desorption rate (the amount of mycotoxins released into the system because they were not retained by the binder) is 20%, 37%, 50%, and 100% for deoxynivalenol, aflatoxin, and zearalenone and ochratoxin. The product therefore has no adsorption capacity in the intestine for the latter (Figures 9 and 10).
[0140] Example 5 - In vivo test 1 on broiler chickens: effect of the product of the invention on performance, metabolism and meat quality
[0141] Study conditions:
[0142] Zootechnical trial on 48 cages of 40 male chickens in a conventional rearing building with a standard feed conversion ratio (J35 CI = 1.50).
[0143] Food:
[0144] Distribution of six feeds (i.e. 8 replicates per feed) to Ross 308 strain broiler chickens for 35 rearing days.
[0145] The food was custom-made with the incorporation of the tested products during the mixing of the raw materials.
[0146] The food does not contain microbial phytase and the raw materials chosen are low in endogenous phytases.
[0147] Products tested: monocalcium phosphates with or without humates. The doses of humates in the product of the invention vary from 1.0 to 2.5%.
[0148] Measurements:
[0149] The following measures were carried out during the rearing process: - Collective weighing on J0, J7, J13, J21 and J28 (total weight of animals / number of individuals) and individual weighing on J35; - GMD (average daily gain) at J7, J13, J21, J28 and J35 (average weight / number of days in the period); - Food consumption at days 7, 13, 21, 28 and 35 (weighing of leftover food at each age, beforehand each bag of food was weighed and identified); - IC (consumption index) at J7, J13, J21, J28 and J35 (ADG / weight of feed consumed for each period); - Blood mineral levels measured on day 35 - Mineral levels in the tibias at day 35 - Quality of the shins: • Latency-to-lie test on D27 • Post-mortem bone strength and resistance - Post-mortem meat quality The study conditions are summarized in Table 5 below.
[0150] [Table 5] In vivo broiler chicken test conditions Breeding characteristics Standard consumption index (CI) Feeding phases: 3 phases: Starter (Day 0-Day 13), Growth (Day 13-Day 28), and Finisher (Day 28-Day 35). Feed characteristics: Ross recommendations: 95% metabolizable energy, protein, and lipids. Phosphorus (P) intake in the form of monocalcium phosphate (MCP): Starter: 100% digestible P in the six feeds. Growth and Finisher: - 100% digestible P with MCP in a positive control feed - 80% digestible P with MCP in a negative control feed - Replacement of MCP with the product of the invention at a rate of 80% digestible P in the last four feeds. Products tested: products of the invention containing 1.0 to 2.5% humates.Zootechnical measures Weight, Average Daily Gain, Feed Consumption, IC Litter Quality Individual Measurements Weight at D35 Metabolism Measurements Blood Doses at D35 Bone Measurements Mineral Doses in Tibias at D35 Latency-to-Lie Test at D27 Post-mortem Bone Strength Measurements Meat Quality Carcass and Cut Weight Evaluation of Wooden Breast and White Stripping Meat pH Number of Animals 8 replicates of 40 males.
[0151] Results of the in vivo study
[0152] The results showed effects on the feed conversion ratio [Fig. 11], quality [Fig. 12] and bone strength [Fig. 13] and meat pH [Fig. 14].
[0153] At a lower dose of digestible P in the feed, the CI is better by -2 points (-1%) with MCPH10 and MCPH15 compared to the positive control (p.val = 0.05) [Fig. 11]. Similarly, the meat pH is closest to the target after 15 minutes of maturation (pH = 6.4) with the addition of MCPH20 (p.val = 0.02) whereas at 7 days of storage (pH = 5.6) this is the case with the addition of MCPH10 (p.val = 0.13) [Fig. 14].
[0154] At the same dose of digestible phosphorus (P) in the feed, tibial fracture strength is 10% and 12% higher, respectively, with MCPH10 and MCPH20 compared to the negative control (p.val. = 0.004) [Fig. 13]. Furthermore, the ash content and the amounts of calcium and phosphorus in these same tibias are 0.4% (p.val. = 0.001), 0.8% (p.val. = 0.004), and 1.7% (p.val. = 0.04) higher, respectively, with MCPH10 compared to the negative control [Fig. 14]. Thus, at the same nutrient quantity, 80% digestible P in the ration provided using the product of the invention results in a better feed conversion ratio (FCR) than with 100% digestible P provided with a standard monocalcium phosphate. Similarly, with the same quantity of nutrients, including digestible P, the product of the invention allows for better results in bone quality and meat preservation.
[0155] Example 6 - In vivo test on broiler chickens: effect of the product of the invention on performance, leg quality and litter
[0156] Study conditions
[0157] Zootechnical trial on 16 cages of 30 male chickens in a conventional rearing building with a minimum prevalence of 70% in pododermatitis and a standard feed conversion ratio (FC = 1.50 at D35 and 1.65 at D42).
[0158] Food:
[0159] Two feeds (8 replicates per feed) were administered to Ross 308 broiler chickens for 42 rearing days. The feed was custom-made with the tested products incorporated during the mixing of the raw materials. At the end of the manufacturing process, a phytase was added on-top to the feed at an equivalent dose of 500 FTU / kg. Test products: monocalcium phosphates with or without humates (Control feed: MCPH0; Test feed: MCPH15).
[0160] Measurements:
[0161] The following measures were carried out during the rearing process: - Collective weighing on J0, J7, J13, J21, J28 and J35 (total weight of animals / number of individuals) and individual weighing on J42; - GMD (average daily gain) at J7, J13, J21, J28, J35 and J42 (average weight / number of days in the period); - Food consumption at J7, J13, J21, J28, J35 and J42 (weighing of leftover food at each age; beforehand each bag of food was weighed and identified); - IC (consumption index) at J7, J13, J21, J28, J35 and J42 (ADG / weight of feed consumed for each period); - Quality of litter at J7, J13, J21, J28, J35 and J42 (litter score according to the ITAVI grid, French poultry technical institute); - Pododermatitis at J21 and J42 (score according to the ITAVI rating grid); - Residual P in the bedding at J21 and J42 (2 samples per cage, one sample halfway between the edge of the cage on the sleeping side and the pipette line and one third between the feeder and the edge of the cage; one sample halfway between the edge of the cage on the sleeping side and the pipette line and two thirds between the feeder and the edge of the cage) by inductively coupled plasma atomic emission spectrometry (ICP-OES) of P after mineralization with hot aqua regia.
[0162] The study conditions are summarized in Table 6 below.
[0163] [Table 6] In vivo broiler chicken test conditions Breeding characteristics: 70% prevalence of pododermatitis. Standard feed conversion ratio (FCR). Feeding phases: 3 phases: Starter (Day 0-Day 13), Growth (Day 13-Day 28) and Finisher (Day 28-Day 42). Feed characteristics: Ross recommendations: 6% metabolizable energy, 10% crude protein, 10% digestible lysine, 6% calcium, 10% phosphorus, 11% Ca / P ratio relative to requirements. Phosphorus supplementation as monocalcium phosphate (MCP). Standard dose (500 FTU / kg) of on-top phytase. Starter: 100% digestible phosphorus in both feeds. Growth and finishing: Replacement of MCP with the product of the invention at a level of 80% digestible phosphorus (22.7% P, 17.0% Ca and 0.0% Na) in one of the two feeds. Products tested: MCPH0 and MCPH15. Zootechnical measurements: Weight, Average Daily Gain, Feed Consumption, Feed Conversion Ratio. Litter quality. Individual measurements: Weight at day 42 and footpad dermatitis measurements. Measurements on litter: Moisture, Phosphorus. Number of animals: 8 replicates of 30 males.
[0164] Results of the in vivo study
[0165] Among the results obtained, significant effects were observed on the consumption index (CI) over the period 0-35 days as illustrated in [Fig. 15].
[0166] This shows that 1TC is significantly lower by 2 points (-1%; p.val = 0.056) over the 0-35 day period with the product of invention (MCPH15) compared to the control MCPH0. This result confirms what had already been observed in the previously presented trial. Furthermore, at the same digestible P dose in the feed, the product The invention allows to significantly reduce (p.val = 0.001) by 14% the quantity of P2O5 in the litter at J42 compared to the supply of a standard monocalcium phosphate ([Fig. 16]).
Claims
Claims
1. A feed raw material for animal nutrition comprising an organo-mineral complex containing feed phosphate and a humic substance, the feed phosphorus being a calcium phosphate and the humic substance being a potassium humate or a sodium humate.
2. Raw material according to claim 1, characterized in that the food phosphate is chosen from monocalcium phosphate, dicalcium phosphate, monobicalcium phosphate, tricalcium phosphate, and mixtures thereof.
3. Raw material according to claim 1, characterized in that the dose of humates in the raw material is between 1.0% and 10.0% by mass.
4. Raw material according to claim 3, characterized in that the dose of humates in the raw material is between 1.0% and 2.5% by mass.
5. A method of manufacturing a food raw material, comprising a step of preparing an aqueous dispersion or solution containing a humic substance, followed by mixing this dispersion or solution with a source of phosphorus and with a source of calcium, the humic substance being a potassium humate or a sodium humate, the source of phosphorus being phosphoric acid, and the source of calcium being chosen from calcium carbonate, quicklime or slaked lime
6. Manufacturing method according to claim 5, characterized in that the potassium humate or the sodium humate is extracted from leonardite.
7. Manufacturing process according to claim 5, characterized in that a mixture of an aqueous solution containing potassium humate or sodium humate, with the phosphorus source and with the calcium source is carried out at a temperature ranging from 50°C to 80°C.
8. Manufacturing process according to claim 5, characterized in that an aqueous solution of potassium humate or sodium humate is mixed with stirring with phosphoric acid, and in that the dispersion obtained is mixed with calcium carbonate.