Method for producing a composition for feed

Abstract

To provide a method for producing a composition for feed containing high-content fatty acid calcium, in which the method has excellent versatility, can make workability efficient, and can improve a generation rate of fatty acid calcium.SOLUTION: A method for producing composition for feed containing fatty acid calcium has: an enzymolysis process (S1) in which triglyceride containing unsaturated fatty acid as constituent fatty acid and lipase are mixed under the presence of water to enzymatically decompose triglyceride; a salt generating process (S2) in which a decomposed product obtained in the enzymolysis process (S1) and calcium hydroxide are mixed to generate fatty acid calcium; a solid-liquid separation process (S3) in which a solid matter is separated from a processed product after the salt generating process (S2); and an antioxidation process (S4) in which the separated solid matter and antioxidative caramel are mixed.SELECTED DRAWING: Figure 1

Description

Technical Field

[0001] The present invention relates to a method for producing a feed composition containing calcium fatty acid.

Background Art

[0002] Conventionally, feed compositions containing triglycerides, fatty acids, etc. have been widely used in feeds for livestock animals such as cows and pigs. These are formulated for the purpose of efficiently supplying energy. Among them, calcium fatty acid, which is a metal salt of fatty acid, is mainly formulated for the purpose of suppressing the decrease in milk fat in dairy cows in summer. In addition, calcium fatty acid containing n-3 fatty acids using linseed oil etc. as raw material oils is formulated in feeds for the purpose of improving the quality by the transfer of n-3 fatty acids to meat quality (cows, pigs, chickens, etc.) and chicken eggs. Calcium fatty acid is, for example, premixed in feeds by feed companies or added to each feed immediately before feeding at each livestock farm.

[0003] As a manufacturing technique for a feed composition containing calcium fatty acid, Patent Document 1 has been proposed. Patent Document 1 describes a method for manufacturing the feed composition, which includes a step of mixing a triglyceride mainly composed of an unsaturated fatty acid, calcium hydroxide, water, caramel having antioxidant properties, and lipase, and a step of reacting the mixture at a temperature of 60°C or lower to produce a composition containing calcium fatty acid. According to this method, it is described that a feed composition with high oxidation stability and excellent odor and palatability can be obtained.

Prior Art Documents

Patent Documents

[0004]

Patent Document 1

Summary of the Invention

Problems to be Solved by the Invention

[0005] In Patent Document 1 mentioned above, calcium fatty acid is obtained by an enzymatic decomposition method using lipase, which is a hydrolytic enzyme for fats and oils. In such an enzymatic decomposition method, the hydrolysis efficiency is affected by the type of lipase and the like, and as a result, the production rate of calcium fatty acid varies. In Patent Document 1 mentioned above, enzymatic decomposition is carried out under alkaline conditions, and since the lipase that can be used is restricted, there is a risk of affecting the hydrolysis efficiency. In addition, alkaline lipase is relatively expensive, and there is room for improvement in terms of versatility.

[0006] Also, in the production method of Patent Document 1 mentioned above, after mixing raw materials including triglyceride, calcium hydroxide, caramel having antioxidant properties, and lipase for about 30 minutes, when the viscosity increased, it was transferred to another container, and the enzymatic decomposition reaction of fats and oils and the production reaction of calcium fatty acid were carried out in the other container over about 30 hours and then solidified. After that, the solidified product was taken out from the container and pulverized to obtain calcium fatty acid. However, such a method is considered to have room for improvement from the viewpoint of workability.

[0007] The present invention has been made in view of such circumstances, and aims to provide a production method that is excellent in versatility, can improve work efficiency, can improve the production rate of calcium fatty acid, and can produce a feed composition containing a high content of calcium fatty acid.

Means for Solving the Problems

[0008] The production method of the feed composition of the present invention is a production method of a feed composition containing calcium fatty acid, and includes an enzymatic decomposition step of mixing a triglyceride containing an unsaturated fatty acid as a constituent fatty acid and lipase in the presence of water to enzymatically decompose the triglyceride, and a salt formation step of mixing the decomposition product obtained in the enzymatic decomposition step and calcium hydroxide to produce calcium fatty acid.

[0009] The lipase is a lipase with non-specific position of the triglyceride. In addition, the enzymatic decomposition step is a step carried out at 30°C to 50°C for 2 hours or more.

[0010] The above manufacturing method is further characterized by having a solid-liquid separation step of separating solids from the processed product after the above salt generation step, and an antioxidant addition step of mixing the separated solids with antioxidant caramel.

[0011] The above solid-liquid separation step is characterized by having a dehydration treatment of dehydrating so that the moisture content of the separated solids becomes 10% by mass to 30% by mass.

[0012] The above salt generation step is characterized by being a step of heating at a temperature near the melting point of the above calcium fatty acid in the presence of antioxidant caramel.

[0013] The above manufacturing method is further characterized by having a solidification step of solidifying the processed product after the above salt generation step, and a pulverization step of pulverizing the solidified processed product.

[0014] The above antioxidant caramel is characterized in that the decrease in absorbance at 517 nm per 1 mg after reacting with a 0.5 mM 1,1-diphenyl-2-picrylhydrazyl (DPPH) ethanol solution at 37°C for 30 minutes is 0.6 to 1.1.

Advantages of the Invention

[0015] The manufacturing method of the feed composition of the present invention has an enzymatic decomposition step of mixing a triglyceride containing an unsaturated fatty acid as a constituent fatty acid and lipase in the presence of water to enzymatically decompose the triglyceride, and a salt generation step of mixing the decomposition product and calcium hydroxide to generate calcium fatty acid. Therefore, the enzymatic decomposition step can be carried out under neutral conditions, and it is not easily restricted by the type of lipase, so it has excellent versatility and a lipase suitable for the hydrolysis efficiency of triglyceride can be used. As a result, the production rate of calcium fatty acid can be improved, and a feed composition containing a high content of calcium fatty acid can be obtained.

[0016] Since the lipase is a lipase with non-specific position for triglycerides and can randomly hydrolyze the ester bonds in triglycerides, the production rate of free fatty acids containing unsaturated fatty acids can be improved (for example, the production rate of free fatty acids in the oil layer after lipase decomposition is about 95 to 97%). In addition, the lipase with non-specific position is generally less expensive than alkaline lipase, and the cost can be reduced. Further, since the enzymatic hydrolysis step is a step carried out at 30 °C to 50 °C for 2 hours or more, the activity of the lipase can be promoted and the enzymatic hydrolysis can be carried out more reliably.

[0017] The production method of the present invention further includes a solid-liquid separation step of separating solids and an antioxidant prevention step of mixing the obtained solids with an antioxidant caramel. Therefore, for example, an operation of taking out the solidified product solidified as in the prior art from the container is not required. In addition, in the case of the prior art, after the reaction solution is poured into another container, the reaction solution remaining in the tank may also solidify, and it may take time to clean the tank, etc., but such cleaning is not required either. As a result, the work efficiency can be improved.

[0018] The solid-liquid separation step has a dehydration treatment for dehydrating so that the water content of the separated solid becomes 10% by mass to 30% by mass, which facilitates the proper execution of the subsequent antioxidant prevention step. Specifically, foaming associated with the addition of the antioxidant caramel during vacuum drying using a double cone or the like can be suppressed, and since it contains 10% by mass or more of water, the antioxidant caramel easily adheres to the particles of calcium fatty acid, and by being uniformly mixed, the antioxidant caramel can be appropriately coated with calcium fatty acid.

[0019] In the salt formation step, by heating at a temperature near the melting point of calcium fatty acid and reacting the fatty acid (including water) after enzymatic hydrolysis with calcium hydroxide to produce calcium fatty acid in a semi-molten state, the production reaction of calcium fatty acid can be completed quickly (for example, within 1 hour). As a result, the work efficiency can be improved.

[0020] Since the above antioxidant caramel has a predetermined antioxidant property in the evaluation of antioxidant property using 1,1-diphenyl-2-picrylhydrazyl (DPPH), even when a triglyceride having a high content ratio of unsaturated fatty acids such as linseed oil is used, the oxidation of unsaturated fatty acids can be effectively prevented.

Brief Description of Drawings

[0021]

Figure 1

Figure 2

Figure 3

Modes for Carrying Out the Invention

[0022] The method for producing a feed composition of the present invention will be described with reference to FIG. 1. FIG. 1 is a flowchart showing an example of a method for producing a feed composition of the present invention. The production method shown in FIG. 1 includes an enzymatic decomposition step (S1), a salt formation step (S2), a solid-liquid separation step (S3), and an antioxidant step (S4). The feed composition obtained by this production method is used for feeds given to livestock animals and the like. Hereinafter, each step will be described in detail.

[0023] [Enzymatic Decomposition Step (S1)] This step is a step of enzymatically decomposing triglyceride using lipase. The triglyceride serving as the raw material oil may have at least one of the constituent fatty acids being an unsaturated fatty acid. Examples of the unsaturated fatty acid include oleic acid, linoleic acid, α-linolenic acid, bis-homo-γ-linolenic acid, arachidonic acid, eicosapentaenoic acid (EPA), docosahexaenoic acid (DHA), and the like. Examples of the raw material oils containing these unsaturated fatty acids include linseed oil, soybean oil, rapeseed oil, corn oil, perilla oil, fish oil, green nut oil, and the like, and these can be used alone or as a mixed oil.

[0024] As the raw material oil or fat, it is preferable that the content ratio of n-3 fatty acids such as α-linolenic acid, EPA, and DHA is 50% by mass or more based on the total constituent fatty acids, and it is more preferable that the content ratio of α-linolenic acid is 50% by mass or more based on the total constituent fatty acids. Specific examples of such raw material oil or fat include linseed oil and perilla oil.

[0025] From another perspective, in the raw material oil or fat, the mass ratio of n-3 fatty acids to n-6 fatty acids (n-3 fatty acids / n-6 fatty acids) in the constituent fatty acids of the raw material oil or fat is preferably 1 to 10, and more preferably 2 to 6.

[0026] Linseed oil is a vegetable oil extracted from flax (Linum usitatissimum) seeds. After extracting oil from flax, linseed oil from which moisture, gum substances, free fatty acids, pigment components, etc. have been removed through degumming, deacidification, decolorization, etc. is commercially available, and such commercial products can be used as the raw material oil or fat. Also, linseed deodorized oil may be used as the linseed oil.

[0027] The lipase used in the S1 step is not particularly limited, and lipases derived from animals, plants, or microorganisms can be used. For example, lipases derived from the genus Candida, Aspergillus, Mucor, Pseudomonas, Burkholderia, etc. can be used. Regarding the positional specificity of triglycerides, lipases include 1,3-position-specific lipases and position-nonspecific lipases. Commercially available products of 1,3-position-specific lipases include, for example, Lipase AK "Amano" (manufactured by Amano Enzyme Inc., derived from Pseudomonas fluorescence), Lipase AS "Amano" (manufactured by Amano Enzyme Inc., derived from Aspergillus niger), Lipase PL (manufactured by Meito Sangyo Co., Ltd., derived from Pseudomonas pseudoalcaligenes), Lipase QLM (manufactured by Meito Sangyo Co., Ltd., derived from Burkholderia ubonensis), etc.

[0028] In the present invention, from the viewpoint of hydrolysis efficiency, it is preferable to use a non-site-specific lipase, that is, a lipase capable of randomly hydrolyzing ester bonds in triglycerides. Such a non-site-specific lipase is liable to be inactivated in an alkaline environment. As the non-site-specific lipase, specifically, a lipase derived from the genus Candida is preferable. As commercially available products, for example, Lipase OF (manufactured by Meito Sangyo Co., Ltd., derived from Candida cylindracea), Lipase AYS "Amano" (manufactured by Amano Enzyme Inc., derived from Candida rugosa), etc. are available.

[0029] The addition amount of lipase in the S1 step is appropriately set according to the activity of the lipase, etc. For example, lipase with a titer of 100 U to 1000 U is added per 1 g of raw material oil and fat, and preferably 300 U to 1000 U of lipase is added. In addition, the lipase is, for example, dissolved in advance while kneading with water to form a lipase solution, and the lipase solution is added to the raw material oil and fat while stirring.

[0030] The addition amount of water in the S1 step (including the water in the lipase solution) is, for example, 0.5 times to 5 times the weight of the raw material oil and fat. Considering the hydrolysis efficiency and handling in subsequent steps, etc., the addition amount of water is preferably 0.5 times to 3 times the weight of the raw material oil and fat, and more preferably 0.5 times to 2 times the weight of the raw material oil and fat.

[0031] The S1 step is preferably carried out at 30°C to 60°C. Within this temperature range, it is excellent in terms of the reaction temperature, activity, thermal stability, etc. of the lipase, and high effects can be expected. More preferably, it is 30°C to 50°C, and still more preferably 30°C to 45°C. The heating time of the S1 step is preferably 2 hours or more, and more preferably 4 hours or more, in order to complete the enzymatic degradation. When using a raw material oil and fat with a high content ratio of unsaturated fatty acids, from the viewpoint of antioxidant protection, the upper limit of the heating time at 30°C to 45°C is preferably about 10 hours. In addition, after the heating time ends, if necessary, the reaction may be continued for a predetermined time without heating.

[0032] Also, in the S1 step, in order to suppress the oxidation of unsaturated fatty acid residues in the raw material oil and fat, an antioxidant may be added as necessary. Examples of the antioxidant include ethoxyquin, dibutylhydroxytoluene (BHT), butylhydroxyanisole (BHA), and the like. These may be used alone or in combination of two or more.

[0033] [Salt formation step (S2)] This step is a step of producing calcium fatty acid using calcium hydroxide. For example, the reaction solution after the S1 step is added while stirring to another reaction tank containing calcium hydroxide and water. Note that water may be used as necessary, and when used, the amount used is, for example, 2 to 10 times the weight of the raw material oil and fat. After adding the entire amount of the reaction solution after the S1 step, it is stirred at room temperature (for example, 25°C) for 10 minutes or more, preferably 1 hour or more. This step is different from the above-described S1 step in that heat is not intentionally applied. The free fatty acid generated in the S1 step reacts with calcium hydroxide, and particles of calcium fatty acid precipitate as solids.

[0034] The molar ratio of calcium hydroxide used in the S2 step is not particularly limited, but is preferably 1.2 to 2.0, more preferably 1.3 to 1.8, based on the raw material oil and fat. The molar ratio of calcium hydroxide is calculated based on the molar ratio determined from the molecular weight of triglyceride (molecular weight 872) calculated based on the composition of the constituent fatty acids of the linseed oil and the weight of the linseed oil used, for example, when linseed oil is used as the raw material oil and fat.

[0035] [Solid-liquid separation step (S3)] This step is a step of separating solids from the treated product after the S2 step. As the means for solid-liquid separation, well-known means for solid-liquid separation can be adopted, and means such as mesh filtration, suction filtration, and centrifugation can be adopted. For example, when performing mesh filtration, it is preferable to use a sieve with 32 meshes (opening size 50 μm) to 100 meshes (opening size 154 μm) as the filter. Note that the separated liquid is treated as waste liquid after pH adjustment and the like.

[0036] The solid matter obtained by the solid-liquid separation means may be directly used in the subsequent step S4, but if necessary, a dehydration treatment may be performed to reduce the moisture content of the solid matter to a predetermined level or less. For example, the moisture content of the solid matter separated by mesh filtration is about 40% by mass, and this solid matter is subjected to a dehydration treatment so that the moisture content becomes 10% to 30% by mass. In order to suppress foaming caused by vacuum drying in the subsequent antioxidant step as much as possible, it is preferable that the moisture content is lower, but since the antioxidant caramel easily adheres to the calcium fatty acid particles and the caramel is uniformly mixed, for example, it is set to 10% by mass or more. The moisture content of the solid matter after the dehydration treatment is preferably 20% to 30% by mass.

[0037] From the viewpoint of antioxidant, the dehydration treatment is preferably carried out under the condition that the product temperature is maintained at 40°C or lower, preferably 25°C to 35°C. As the dehydration treatment, a method using various drying devices, suction filtration, centrifugal separation, etc. may be performed. For example, when using a vacuum drying device such as an evaporator, it is carried out at a degree of vacuum of 10 Torr to 50 Torr and a heating temperature (hot water bath temperature) of 50°C to 90°C. In addition, drying may be performed by heating using a conduction heat transfer type rotary drying device such as a double cone. In the above dehydration treatment, a plurality of methods may be combined. For example, after centrifugal separation, drying by a double cone can be performed.

[0038] The moisture content of the solid matter can be calculated by the drying loss method (method described in the feed analysis standard). The above dehydration treatment is completed based on the calculated moisture content.

[0039] In addition, as the solid-liquid separation means, when performing suction filtration or centrifugal separation instead of mesh filtration, the treatment can be continued until the moisture content of the solid matter becomes 30% by mass or less within the above numerical range while separating the solid matter.

[0040] [Antioxidant step (S4)] This step is to obtain a feed composition by mixing and stirring the solid separated in step S3 with the antioxidant caramel. The antioxidant caramel is, for example, a caramel having antioxidant properties obtained by heating an aqueous solution of a monosaccharide such as pentose or hexose in the presence of a basic compound under predetermined conditions. When adding the antioxidant caramel to the solid, it is preferable to preheat the antioxidant caramel to about 40°C to make it have fluidity before adding it.

[0041] Also, the addition amount of the antioxidant caramel is preferably 1% to 10% by mass, more preferably 4% to 10% by mass, based on the weight of calcium fatty acid. The weight of calcium fatty acid can be obtained, for example, by calculating the moisture content from the solid after the dehydration treatment in step S3 by the drying loss method (the method described in the feed analysis standard), and subtracting the moisture amount from the weight of the solid.

[0042] Examples of the monosaccharide used as the raw material of the antioxidant caramel include glucose, xylose, galactose, fructose, etc. Among these, glucose, which is easily available and inexpensive, is preferable. Examples of the basic compound include alkali metal carbonates such as sodium carbonate and potassium carbonate, alkali metal hydroxides such as sodium hydroxide and potassium hydroxide, alkali metal hydrogen carbonates such as sodium hydrogen carbonate and potassium hydrogen carbonate, sodium salts and ammonium salts of organic acids such as acetic acid and citric acid, and ammonium hydroxide. As the antioxidant caramel used in the present invention, it is preferable to use the caramel obtained by heat-treating glucose and sodium carbonate.

[0043] The antioxidant caramel can be obtained, for example, by heating for about 1 hour to 10 hours in the presence of 1 part to 10 parts by mass of a basic compound with respect to 100 parts by mass of an aqueous solution of 75% to 95% by mass of monosaccharide. The heating temperature is preferably 100°C or higher, more preferably 120 to 150°C. The pH of the obtained caramel is preferably 5 or less.

[0044] The antioxidant property of the obtained caramel can be evaluated by the following method using, for example, 1,1-diphenyl-2-picrylhydrazyl (DPPH). First, dissolve the above caramel in a predetermined amount of ethanol, add a 0.5 mM DPPH ethanol solution thereto, and hold at 37°C for 30 minutes. Then, measure the absorbance at 517 nm and create a regression line of the amount of caramel and the decrease in absorbance due to the addition of caramel. From this regression line, the decrease in absorbance per 1 mg of caramel is determined, and this value can be used to evaluate the antioxidant property of the caramel. This value is preferably 0.6 to 1.1.

[0045] In the S4 step, the mixing of the solid and the antioxidant caramel and the drying of the treated product may be performed simultaneously. For example, it can be mixed and stirred under a predetermined degree of reduced pressure and predetermined temperature conditions. In this case, it is preferably performed under the condition that the product temperature is maintained at 40°C or lower, preferably 25°C to 35°C. The degree of reduced pressure is preferably 10 Torr to 50 Torr, and the heating temperature is preferably 50°C to 90°C.

[0046] In the S4 step, the mixing and drying may be performed as separate processes instead of simultaneously. In this case, the mixing of the solid and the antioxidant caramel is performed at room temperature (for example, 25°C) without heating. Further, the subsequent drying is performed by reduced-pressure drying under conditions that can maintain the product temperature at 40°C or lower. For example, it is dried at a reduced pressure of 10 Torr to 50 Torr and a heating temperature of 50°C to 90°C.

[0047] The drying in the S4 step is performed until the moisture content of the treated product reaches a predetermined moisture content (for example, 13.5% by mass). The feed composition obtained by drying may be pulverized into a powder by a hammer mill pulverizing device or the like, if necessary.

[0048] In the manufacturing method of FIG. 1, a preferred form for the S3 and S4 steps is as follows: in the solid-liquid separation step (S3), first, solid-liquid separation is performed to obtain a solid (water content: about 40% by mass), and then, using a centrifuge or an evaporator, etc., the water content of the solid is dehydrated to 10% to 30% by mass. After that, in the antioxidant addition step (S4), an antioxidant caramel is added and the solid is further dried until the water content of the solid becomes 10% to 13.5% by mass. In this case, the solid-liquid separation step has a dehydration treatment, and the antioxidant addition step includes a drying step.

[0049] Specific examples of the above preferred form are shown below. The calcium fatty acid produced in the salt formation step (S2) is put into a double cone in a state containing water. This double cone has a mesh attached to the outlet, and solid-liquid separation and dehydration (drying) are performed by this double cone. First, the solid is separated by solid-liquid separation using the mesh, and then the solid is dried in the double cone. And at the stage where the water content is dried to 10% to 30% by mass, while rotating the double cone without releasing the vacuum, an antioxidant caramel is added through a nozzle, and while mixing the caramel with the particles of calcium fatty acid, it is dried until the water content becomes 10% to 13.5% by mass. By performing the S3 and S4 steps in such a series of processes, further efficiency improvement of workability can be achieved.

[0050] FIG. 2 is a flowchart showing another example of the manufacturing method of the feed composition of the present invention. The manufacturing method shown in FIG. 2 includes an enzymatic decomposition step (S1), a salt formation step (S2'), a solidification step (S5), and a pulverization step (S6). Hereinafter, each step will be described. The enzymatic decomposition step (S1) is the same step as the enzymatic decomposition step of FIG. 1 described above, and the description thereof will be omitted.

[0051] [Salt Formation Step (S2')] This step is a step of producing calcium fatty acid using calcium hydroxide. For example, the oil layer (including water) of the reaction solution in the S1 step is transferred to another reaction tank, and calcium hydroxide, water, and antioxidant caramel are added thereto while stirring. Note that water may be used as necessary, and the amount used, when used, is, for example, 0.001 times to 1.0 times the weight of the raw material oil and fat. In addition, the molar ratio of calcium hydroxide used in this step, the addition amount of antioxidant caramel, the antioxidant property of antioxidant caramel, etc. can appropriately apply the above-described numerical ranges. After adding calcium hydroxide, water, and antioxidant caramel to the oil layer (including water) of the reaction solution after the S1 step, it is stirred at a temperature near the melting point of calcium fatty acid for 1 hour or less, preferably for 10 minutes to 30 minutes.

[0052] The S2’ step is carried out under predetermined heating conditions, different from the S2 step in the manufacturing method of FIG. 1 described above. The temperature near the melting point of the above calcium fatty acid is, for example, within the range of ±30°C of the melting point of calcium fatty acid. This calcium fatty acid refers to at least one of the calcium fatty acids derived from the constituent fatty acids of the raw material oil and fat. For example, when linseed oil is used as the raw material oil and fat, the S2’ step is carried out by heating at 70°C to 200°C. More preferably, it is carried out by heating at 90°C to 160°C. By reacting while controlling the reaction temperature in the presence of a small amount of water, calcium fatty acid can be produced in a semi-molten state, and the reaction can be completed promptly.

[0053] [Solidification step (S5)] The processed product after the S2’ step is taken out into another container and cooled to solidify. For example, it is left standing at room temperature for 1 hour to 15 hours. The prior art performs the enzymatic decomposition reaction of fats and oils and the production reaction of calcium fatty acid in a separate container, and allows it to stand for a long time (about 30 hours). In contrast, in the manufacturing method of FIG. 2, before the S5 step, the enzymatic decomposition reaction of fats and oils and the production reaction of calcium fatty acid are completed step by step, and this S5 step is performed to solidify the semi-molten calcium fatty acid. That is, the purposes after transferring to a separate container are different between the prior art and the manufacturing method of FIG. 2. As a result, the standing time of the S5 step can be made shorter than the standing time of the prior art (about 30 hours), and the work efficiency can be improved.

[0054] [Grinding step (S6)] The solid obtained in the S5 step is ground into a powder by a hammer mill or the like.

[0055] In the manufacturing method of the present invention, in addition to raw material fats and oils, lipase, calcium hydroxide, water, and antioxidant caramel, other additives may be appropriately added. For example, flavor improvers such as molasses, emulsifiers such as glycerin fatty acid esters, fungicides such as propionic acid, sweeteners such as sodium saccharin, and fragrances may be appropriately added.

[0056] The feed composition obtained by the above manufacturing method is given to livestock animals as it is, or is blended with other feed compositions and given as feed. The obtained feed composition preferably contains 52% by mass or more of calcium fatty acid based on the total amount of the composition, and more preferably 55% by mass or more.

[0057] In addition, the obtained feed composition also has excellent oxidation stability. The peroxide value (POV) of the feed composition immediately after production is 5 or less, preferably 3 or less, and more preferably 1 or less.

Example

[0058] Example 1 600 g of linseed oil (deodorized oil) was added to a reaction vessel, and while stirring, a lipase solution in which 345 U of lipase OF (manufactured by Meito Sangyo Co., Ltd.) per 1 g of linseed oil was dispersed in 420 g of water (0.7 times the weight of linseed oil) was added to the reaction vessel, and the mixture was stirred and mixed at 40 °C for 6 hours or more. In another reaction vessel, 1634 g of water and 81.58 g of calcium hydroxide (molar ratio of 1.5 or more to linseed oil) were stirred and mixed, and the above reaction solution containing lipase was added in small portions until the total amount was added, and the mixture was stirred and mixed at 25 °C for 6 hours or more. After stirring, solid-liquid separation was performed using a 100-mesh filter, and the solid matter was separated. The separated liquid was treated as waste liquid.

[0059] The water content of the obtained solid was about 40% by mass. This solid was dehydrated in an evaporator under the conditions of a vacuum of 10 Torr to 20 Torr and a hot bath temperature of 85 °C so that the product temperature was maintained at 27 °C to 35 °C until the water content became 25% by mass to 28% by mass. Subsequently, an antioxidant caramel (6.5% by mass based on the solid weight of calcium fatty acid) preheated to about 40 °C was added to the dehydrated solid, and mixing and drying were performed under reduced pressure. Specifically, mixing and drying were performed in an evaporator under the conditions of a vacuum of 10 Torr to 20 Torr and a hot bath temperature of 85 °C so that the product temperature was maintained at 27 °C to 35 °C until the water content became 12% by mass to 13.5% by mass, and a feed composition was obtained. The obtained feed composition was tea-like granular (see Fig. 3(a)).

[0060] The antioxidant caramel used in Example 1 was prepared by mixing 72.5 parts by mass of glucose, 4.5 parts by mass of sodium carbonate as a basic compound, and 23 parts by mass of water, reacting at 130 °C for 3 hours, and then adding 23 parts by mass of water to adjust the viscosity. The antioxidant property of the antioxidant caramel was 1.064.

[0061] The weights of moisture, crude lipid, and ash of the obtained feed composition were measured by the following methods, respectively, and the mass% with respect to the total amount of the feed composition was calculated. The results are shown in Table 1. <Moisture> Accurately weigh 2 g to 5 g of the feed composition into a glass beaker (previously dried and accurately weighed), add 15 g of sea sand thereto, mix well by stirring, dry at 105 ± 2 °C for 3 hours, allow to cool in a desiccator, accurately weigh the weight, and determine the weight of water from the weight difference before and after drying. <Crude lipid> The crude lipid was determined using the acid decomposition diethyl ether extraction method. By measuring the acid value of the crude lipid, the total amount of free fatty acids (Ca-bound type), triacylglycerol (TG), diacylglycerol (DG), and monoacylglycerol (MG) was determined. In addition, the content of free fatty acids not bound to Ca was determined by adding an ether-ethanol mixed solution (2:1) to the feed composition, shaking vigorously, filtering using filter paper, adding several drops of phenolphthalein indicator to the filtrate, and titrating this with 0.1 N potassium hydroxide-ethanol solution. <Ash> Accurately weigh 2 g to 5 g of the feed composition, place it in a crucible, gently heat and carbonize it, then heat and ashing at 550 °C to 600 °C for 4 hours, allow to cool in a desiccator, accurately weigh the weight, and determine the weight of ash.

[0062] <Calcium fatty acid formation rate> Taking the formation rate when all constituent fatty acids of the linseed oil (deodorized oil) used as the raw material oil became calcium fatty acid as 100%, the formation rate of calcium fatty acid (Ca-bound free fatty acid) in the feed composition was calculated.

[0063] Example 2 Add 40 kg of linseed oil (deodorized oil) to the reaction tank, and while stirring, add to the reaction tank a lipase solution in which 345 U of lipase OF (manufactured by Meito Sangyo Co., Ltd.) per 1 g of linseed oil is dispersed in 40 kg of water (equivalent to the weight of linseed oil), and mix and stir at 30 °C for 6 hours or more. Then, stop stirring and heating, allow to stand and separate for 15 hours, and discharge 36.8 kg of the aqueous layer.

[0064] The oil layer remaining in the reaction tank (a lipase-treated liquid containing linseed oil fatty acid and containing water) was transferred to a reaction tank for calcium fatty acid production, and antioxidant caramel (5.25% by mass based on the solid weight of the calcium fatty acid to be produced) pre-heated to 30 °C was added thereto. Further, while stirring, the product temperature was raised to 95 °C, and then 5.48 kg of calcium hydroxide (molar ratio of 1.5 or more with respect to linseed oil) was added. Air was enclosed in the reaction tank and stirring was continued at about 100 °C for 25 minutes while applying pressure to carry out the production reaction of calcium fatty acid in a semi-molten state. After the reaction, the semi-molten calcium fatty acid was discharged from the lower part of the reaction tank and collected in a tray. Since the recovered calcium fatty acid solidifies as the product temperature decreases, it was left standing at room temperature for 15 hours. Thereafter, the solidified calcium fatty acid was crushed into blocks and then pulverized using a hood mixer to obtain a feed composition. The obtained feed composition was in the form of a tea-colored powder (see Fig. 3(b)). For this feed composition as well, the weights of moisture, crude lipid, and ash were measured in the same manner as in Example 1.

[0065] Comparative Example To 78 parts by mass of linseed oil (deodorized oil), 10.6 parts by mass of calcium hydroxide was added and mixed and stirred in a mixing tank. To this mixture, 4 parts by mass of antioxidant caramel produced in the same manner as above, 7.4 parts by mass of water, and 0.04 parts by mass of lipase PL (manufactured by Meito Sangyo Co., Ltd.) were added, the liquid temperature was raised to 40 °C, and further stirred for 30 minutes. A block-shaped solid was taken out from the mixing tank and placed in a container. Thereafter, it was left standing at room temperature for 30 hours, the solidified mixture was taken out from the container, and pulverized by a hammer mill pulverizing device. As a result, a yellowish powder feed composition was obtained (see Fig. 3(c)). Note that lipase PL is an alkali-resistant lipase. For this feed composition as well, the weights of moisture, crude lipid, and ash were measured in the same manner as in Example 1. The results are shown in Table 1.

[0066]

Table 1

[0067] As shown in Table 1, the moisture values of the feed compositions of Examples 1 to 2 and the Comparative Example were approximately 10% by mass. Regarding free fatty acids (Ca-bound type), the feed compositions of Examples 1 to 2 were higher than those of the feed composition of the Comparative Example, and it was found that a feed composition with a higher content of calcium fatty acid could be obtained. Also, regarding the separately calculated calcium fatty acid production rate, the Comparative Example was 76.9%, while Example 1 was 80.7%, and the result of Example 1 was superior. Here, the manufacturing method according to Example 1, different from the Comparative Example (prior art), can use a non-site-selective lipase by performing the enzymatic decomposition step and the salt formation step step by step, and thereby the hydrolysis efficiency is considered to have increased. Also, the manufacturing method according to Example 1, although there is a step of separating solids by a solid-liquid separation step, does not require the operation of taking out the solidified product from the container as in the prior art, and the workability is good even in mass production.

[0068] On the other hand, the calcium fatty acid production rate of Example 2 was 75.0%. However, the manufacturing method according to Example 2 can perform the calcium fatty acid production reaction in a short time by the semi-melting method, and it is considered that the calcium fatty acid production rate can be further increased by extending the reaction time by about 5 to 10 minutes. Also, in Example 2, since the reaction can be completed in the reaction tank for producing calcium fatty acid, it becomes possible to pulverize immediately at the stage of solidification by air cooling after discharge, so that the working time can be shortened compared to the prior art.

[0069] <Peroxide value (POV)> The POV immediately after the production of the feed composition of Example 1 and the POV after storage in an aluminum pouch bag in a warehouse (25 °C) for 7 days were measured respectively. The measurement was in accordance with the "Standard Oil Analysis Test Method" edited by the Japanese Oil Chemists' Society. As a result, the POV immediately after production was 0.27, and the POV after 7 days was 0.49. It was found that the POV immediately after production and after 7 days were both 1 or less, and it had excellent oxidation stability. On the other hand, when Example 2 also measured the POV in the same manner as Example 1, the POV immediately after production and after 7 days was 0.

Industrial Applicability

[0070] The manufacturing method of the feed composition of the present invention includes an enzymatic decomposition step and a salt formation step, can improve the production rate of calcium fatty acid, and can produce a feed composition containing a high content of calcium fatty acid. Therefore, it can be suitably used as a manufacturing method of a feed composition in the livestock field.

Claims

1. A method for producing a feed composition containing calcium fatty acid, comprising: an enzymatic decomposition step of mixing a triglyceride containing an unsaturated fatty acid as a constituent fatty acid and lipase in the presence of water to enzymatically decompose the triglyceride; and a salt formation step of adding and mixing calcium hydroxide and antioxidant caramel to the decomposition product obtained in the enzymatic decomposition step to produce calcium fatty acid, wherein the lipase is a position-nonspecific lipase of the triglyceride, and the salt formation step is a step of heating at a temperature near the melting point of the calcium fatty acid in the presence of the antioxidant caramel. A method for producing a feed composition, characterized in that.

2. The method for producing a feed composition according to claim 1, wherein the enzymatic decomposition step is carried out at 30°C to 50°C for 2 hours or more.

3. The method for producing a feed composition according to claim 1 or claim 2, characterized in that the production method further comprises a solidification step of solidifying the treated product after the salt formation step and a pulverization step of pulverizing the solidified treated product.

4. The antioxidant caramel has a decrease in absorbance at 517 nm per 1 mg of 0.6 to 1.1 after reacting with a 0.5 mM 1,1-diphenyl-2-picrylhydrazyl (DPPH) ethanol solution at 37°C for 30 minutes. A method for producing a feed composition according to any one of claims 1 to 3, characterized in that.

Images