Preparation method of aquatic feed based on coordination of rare earth elements and alpha-starch structure regulation and control
The method of preparing rare earth-α-starch composite microcapsules solves the problem of the easy deactivation of rare earth elements in eel feed, realizes the efficient digestion and absorption of eel feed and improves intestinal health, reduces environmental pollution, and forms a stable intestinal targeted sustained release effect.
Patent Information
- Application Number
- CN202511785436.0
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-12-01
- Publication Date
- 2026-01-23
AI Technical Summary
Existing eel feeds are insufficient in improving digestive efficiency and gut health. Rare earth elements are easily degraded during processing and lack targeted release mechanisms, resulting in low bioavailability. Current technologies lack a complex functional system that combines nutritional optimization, gut regulation, and immune enhancement.
A rare earth-α-starch composite microcapsule preparation method was adopted. Through plasma activation and dynamic Schiff base cross-linking, the physical encapsulation and chemical coordination synergistic effect of rare earth and α-starch were achieved to form a stable microcapsule structure, which improved processing stability and intestinal targeted sustained release effect.
It significantly improves the digestion, absorption, and growth performance of aquatic animals, enhances gut health, reduces nitrogen and phosphorus emissions and antibiotic dependence, and achieves efficient utilization of eel feed.
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Abstract
Description
TECHNICAL FIELD
[0001] The present application relates to the technical field of aquatic feed, in particular to a preparation method of aquatic feed based on synergistic regulation of rare earth elements and α-starch structure. BACKGROUND
[0002] As an important high-value aquatic farming species in China, the growth performance and meat quality of eels are directly related to the nutritional ratio and digestive utilization rate of feed. At present, the feed widely used in the eel farming industry is mainly formulated with high protein and high energy, and the core design idea is to meet the nutritional needs of eel rapid growth by increasing the addition amount of protein and energy substances. In terms of feed function optimization, the existing technology mainly focuses on a single synergistic factor: on the one hand, some studies attempt to add antibiotics, probiotics or enzyme preparations to the feed to improve the intestinal microecological environment of eels and increase the activity of digestive enzymes, but the abuse of antibiotics can easily lead to the emergence of drug-resistant strains, pollution of the water environment and product drug residues, and probiotics have the defects of poor storage stability and being greatly affected by the feed processing technology; on the other hand, in order to optimize the energy structure of the feed, the industry often uses ordinary starch as the energy source, but ordinary starch has low gelatinization degree and poor compatibility with other nutritional ingredients, resulting in low feed conversion rate and the inability to achieve the protection and controlled release of functional ingredients. In addition, regarding the application of rare earth elements in aquatic feed, the existing technology is limited to the direct addition of a single rare earth ion, which mainly utilizes its activation effect on enzyme activity to improve digestion efficiency, but due to the active chemical properties of rare earth elements, they are easily reacted with other ingredients during the feed processing process and lose their effectiveness, and lack a targeted release mechanism, resulting in low bioavailability and difficulty in fully exerting their comprehensive effects of antibacterial, anti-inflammatory and immune regulation; as a modified starch, α-starch has been proven to have good water solubility, gelatinization properties and inclusion capacity, and is used in the fields of food and medicine for the stabilization and slow release of active ingredients, but it has not been applied in eel feed in combination with rare earth elements, and a composite functional system with nutritional optimization, intestinal regulation and immune enhancement has not been formed. Moreover, the development of existing eel feed mainly focuses on the improvement of growth performance, and lacks systematic consideration of nutritional conversion, intestinal health and ecological environmental protection, and has not formed a functional feed product that can be applied on a large scale, has a clear synergistic mechanism and safety guarantee, and the degree of related technology transformation and industrialization is low, which needs to be improved. SUMMARY
[0003] Therefore, the purpose of the present application is to provide a preparation method of aquatic feed based on synergistic regulation of rare earth elements and α-starch structure, so as to improve the utilization rate of aquatic feed and enhance the health regulation effect. The specific scheme is as follows: A preparation method of aquatic feed based on synergistic regulation of rare earth elements and α-starch structure, comprising the following steps: Step 1, mixing: fish meal, soybean meal, mixed filler, compound vitamins, minerals are put into the mixer for stirring and mixing to obtain a basic raw material mixture; Step 2, adding: rare earth-α-starch composite microcapsules, compound prebiotics and oil are sequentially added to the basic raw material mixture, and are mixed, stirred and uniformly dispersed to obtain a functional mixture; Step 3, granulation: the functional mixture is treated by an extruder to obtain feed pellets; The mass ratio of the fish meal, soybean meal, mixed filler, compound vitamins, minerals, rare earth-α-starch composite microcapsules, compound prebiotics and oil is 38-42:16-19:26-32:0.6-0.9:1.2-1.8:9.73-12.245:0.8-1.2:6-7; The rare earth-α-starch composite microcapsules are obtained by coating α-starch with amino modification and rare earth compound cross-linking.
[0004] Preferably: the α-starch is potato α-starch, and the molecular weight is 200-300 million Da, the amino modification includes steps ① low temperature plasma treatment of potato α-starch, and the vacuum degree of the low temperature plasma treatment is controlled to be 0.05-0.08 MPa, the power is 80-120 W, and the treatment time is 15-25 min, and the active starch is obtained under the mixed gas of Ar and oxygen with a volume ratio of 3:1; step ② mixing the active starch with 5% D-glucosamine hydrochloride solution according to a mass ratio of 1:3.8-4.2, and controlling the pH to be 8.5-9.0 and the temperature to be 55-60℃ constant temperature stirring for 2-3 h, and then filtering and drying to obtain amino α-starch with a mass grafting rate of 8-12 wt%.
[0005] Preferably: the rare earth compound is La(NO3)3·6H2O and Ce(NO3)3·6H2O with a mass ratio of 1:0.9-1.05.
[0006] Preferably, the cross-linking coating comprises the following steps: ① 0.03-0.045 parts by mass of rare earth complex is dissolved in deionized water to obtain a rare earth solution with a mass concentration of 6%, and then 0.3-0.5 parts of an active assistant is added to the rare earth solution, and after stirring, the pH is adjusted to 5.5-6.0 to obtain a precursor solution; ② 9-11 parts by mass of amino-modified α-starch is mixed with deionized water at a mass ratio of 1:3.3-3.6, and the temperature is controlled at 60-65°C and the precursor solution is added, and an emulsion is obtained by high-speed shearing; ③ 0.4-0.7 parts of a dynamic cross-linking agent is added to the emulsion, and the temperature is controlled at 45-50°C and stirred for 90-120 min to obtain a dynamic cross-linking coated starch solution; ④ 0.95-1.05 parts by mass of a plasticizer is added to the dynamic cross-linking coated starch solution, and after stirring, spray drying and washing, the finished product of rare earth-α-starch composite microcapsules is obtained.
[0007] Preferably, the active assistant is D-glucosamine hydrochloride, the dynamic cross-linking agent is chitosan-g-glutaraldehyde graft, and the plasticizer is glycerol.
[0008] Preferably, the high-speed shearing is controlled at a speed of 2000-2100 r / min for 28-30 min.
[0009] Preferably, the spray drying is controlled at an inlet air temperature of 160-170°C, an outlet air temperature of 70-80°C, and a feeding speed of 5-8 mL / min; the washing is carried out with anhydrous ethanol; the particle size of the finished product of the rare earth-α-starch composite microcapsules is 8-15 μm, the embedding rate is ≥95%, and the coordination bonding rate is ≥75%.
[0010] Preferably, the mixed filler is bran and oat flour at a mass ratio of 2-2.2:1; the complex vitamin is VA / VD / VE complex vitamin; and the mineral is calcium / phosphorus / zinc complex mineral.
[0011] Preferably, the complex prebiotic is fructooligosaccharide and inulin at a mass ratio of 1:0.95-1.
[0012] Preferably, the oil is fish oil and / or soybean oil.
[0013] It can be known from the above scheme that the application provides a water product feed preparation method based on rare earth element synergistic alpha-starch structure regulation. The water product feed preparation method based on rare earth element synergistic alpha-starch structure regulation realizes the physical embedding and chemical coordination synergistic effect of the rare earth and alpha-starch by introducing active groups through plasma activation and synergistically constructing double combination with dynamic Schiff base cross-linking, so as to improve the processing stability of the water product feed based on rare earth element synergistic alpha-starch structure regulation and achieve the purpose of intestinal targeting and slow release, significantly improve the digestion and absorption and growth performance of aquatic animals, improve intestinal health, and at the same time reduce nitrogen and phosphorus emissions and antibiotic dependence. DETAILED DESCRIPTION
[0014] The technical solutions in the embodiments of the application will be described below in a clear and complete manner. Obviously, the described embodiments are only part of the embodiments of the application, rather than all the embodiments. Based on the embodiments in the application, all other embodiments obtained by those skilled in the art without creative labor fall within the scope of protection of the application.
[0015] It should be noted that the fish meal, soybean meal, mixed filler, compound vitamin, mineral substance, compound prebiotic and oil in the embodiments of the application are commercially available and will not be described here. Specifically, the mixed filler is composed of bran and oat flour in a mass ratio of 2-2.2:1. The compound vitamin is VA / VD / VE compound vitamin. The mineral substance is calcium / phosphorus / zinc compound mineral substance. The compound prebiotic is composed of fructooligosaccharide and inulin in a mass ratio of 1:0.95-1. The oil is fish oil and / or soybean oil. In the embodiments of the application, the mass ratio of fructooligosaccharide and inulin in the compound prebiotic is 1:1. The mass ratio of bran and oat flour in the mixed filler is 2:1. At the same time, the particle size of the rare earth-alpha-starch composite microcapsule of the finished product obtained in the embodiments of the application is 8-15 μm, the embedding rate is ≥95%, and the coordination combination rate is ≥75%.
[0016] The water product feed preparation method based on rare earth element synergistic alpha-starch structure regulation will be described in detail below.
[0017] The water product feed preparation method based on rare earth element synergistic alpha-starch structure regulation comprises the following steps: Step 1, mixing: fish meal, soybean meal, mixed filler, compound vitamin and mineral substance are put into a mixer and stirred and mixed to obtain a basic raw material mixture; Step 2, adding: rare earth-alpha-starch composite microcapsules, compound prebiotic and oil are sequentially added to the basic raw material mixture, and the mixture is mixed and stirred and uniformly dispersed to obtain a functional mixture; Step 3, granulation: the functional mixture is treated by an extruder to obtain feed particles; The mass ratio of the fish meal, soybean meal, mixed filler, compound vitamin, mineral, rare earth-α-starch composite microcapsule, compound prebiotic and oil is 38-42:16-19:26-32:0.6-0.9:1.2-1.8:9.73-12.245:0.8-1.2:6-7.
[0018] The rare earth-α-starch composite microcapsule is obtained by amino modification and cross-linking coating of α-starch. It is noted that the α-starch is potato α-starch, and the molecular weight is 200-300 thousand Da. The rare earth complex is La(NO3)3·6H2O and Ce(NO3)3·6H2O with a mass ratio of 1:0.9-1.05.
[0019] The amino modification includes the following steps: ① low-temperature plasma treatment of potato α-starch, and control of the vacuum degree of the low-temperature plasma treatment at 0.05-0.08 MPa, the power at 80-120 W and the treatment time at 15-25 min to obtain active starch under a mixed gas of Ar and oxygen with a volume ratio of 3:1; ② mixing of the active starch and 5% D-glucosamine hydrochloride solution with a mass ratio of 1:3.8-4.2, control of the pH at 8.5-9.0 and the temperature at 55-60℃, constant temperature stirring for 2-3 h, and then filtration and drying to obtain amino-modified α-starch with a mass grafting rate of 8-12 wt%.
[0020] The cross-linking coating includes the following steps: ① dissolving 0.03-0.045 parts of the rare earth complex in deionized water to obtain a rare earth solution with a mass concentration of 6%, adding 0.3-0.5 parts of an active aid to the rare earth solution, stirring uniformly, adjusting the pH to 5.5-6.0 to obtain a precursor solution; ② mixing 9-11 parts of the amino-modified α-starch with deionized water with a mass ratio of 1:3.3-3.6, controlling the temperature at 60-65℃ and adding the precursor solution, and obtaining an emulsion by high-speed shearing; ③ adding 0.4-0.7 parts of a dynamic cross-linking agent to the emulsion, controlling the temperature at 45-50℃ and stirring for 90-120 min to obtain a dynamic cross-linking coated starch solution; ④ adding 0.95-1.05 parts of a plasticizer to the dynamic cross-linking coated starch solution, and then stirring, spray drying and washing in sequence to obtain the finished product of the rare earth-α-starch composite microcapsule.
[0021] The active assistant used in the cross-linking coating is D-glucosamine hydrochloride, and the plasticizer is glycerol, both of which are commercially available and will not be described here. The dynamic cross-linking agent is chitosan-g-glutaraldehyde graft, which is obtained by adding chitosan with a mass-volume ratio of 1 g:100 mL into 1% acetic acid aqueous solution, controlling the temperature to be 50°C and stirring until completely dissolved, then adding 25% glutaraldehyde solution with a mass ratio of 10:1 to chitosan, controlling the pH to be 5.0-6.0, and stirring at a constant temperature of 45°C for 2h. The high-speed shearing is controlled at a speed of 2000-2100r / min for 28-30min. The spray drying is controlled at an inlet temperature of 160-170°C, an outlet temperature of 70-80°C, and a feeding speed of 5-8mL / min. The washing is performed using anhydrous ethanol.
[0022] Example one A water product feed preparation method based on rare earth element synergistic α-starch structure regulation, comprising the following steps: Step 1, mixing: put fish meal, soybean meal, mixed filler, compound vitamin, mineral into the mixer and stir to mix, to obtain a basic raw material mixture; Step 2, adding: sequentially add rare earth-α-starch composite microcapsules, compound prebiotics and oil to the basic raw material mixture, mix and disperse uniformly to obtain a functional mixture; Step 3, granulation: the functional mixture is treated by an extruder to obtain feed granules; Wherein, the mass ratio of fish meal, soybean meal, mixed filler, compound vitamin, mineral, rare earth-α-starch composite microcapsules, compound prebiotics and oil is 42:19:32:0.9:1.8:9.85:1.2:7.
[0023] The rare earth-α-starch composite microcapsules are obtained by amino modification of α-starch and cross-linking coating of rare earth complex. It should be noted that the α-starch is potato α-starch, and the molecular weight is 20-30 million Da. The rare earth complex is La(NO3)3·6H2O and Ce(NO3)3·6H2O with a mass ratio of 1:0.9.
[0024] The amino modification includes step ① low temperature plasma treatment of potato α-starch, and controlling the vacuum degree of low temperature plasma treatment to be 0.05MPa, the power to be 80W and the treatment time to be 25min, obtaining active starch under the mixed gas of Ar and oxygen with a volume ratio of 3:1; step ② mixing the active starch with 5% D-glucosamine hydrochloride solution with a mass ratio of 1:3.8, controlling the pH to be 8.5 and the temperature to be 55°C constant temperature stirring for 2h, then filtering and drying to obtain amino α-starch with a mass grafting rate of 8.36wt%.
[0025] The cross-linking coating comprises the following steps: ① dissolving 0.03 parts of rare earth complex in deionized water by mass fraction to obtain a rare earth solution with a mass concentration of 6%, then adding 0.3 parts of an active assistant to the rare earth solution, uniformly stirring, and adjusting the pH to 5.5 to obtain a precursor solution; ② mixing 9 parts of amino-modified α-starch with deionized water in a mass ratio of 1:3.6, controlling the temperature to be 60°C, and adding the precursor solution to obtain an emulsion through high-speed shearing; ③ adding 0.4 parts of a dynamic cross-linking agent to the emulsion, controlling the temperature to be 45°C, and stirring for 120 min to obtain a dynamic cross-linking coated starch solution; and ④ adding 0.95 parts of a plasticizer to the dynamic cross-linking coated starch solution by mass fraction, and then obtaining the finished product of rare earth-α-starch composite microcapsules through stirring, spray drying, and washing in sequence.
[0026] In the cross-linking coating, the active assistant is D-glucosamine hydrochloride, and the plasticizer is glycerol, both of which are commercially available and will not be described here. The dynamic cross-linking agent is a chitosan-g-glutaraldehyde graft, which is obtained by adding 1 g of chitosan to 100 mL of 1% acetic acid aqueous solution, controlling the temperature to be 50°C, stirring until completely dissolved, then adding 25% glutaraldehyde solution with a chitosan mass ratio of 10:1, controlling the pH to be 5.0, and stirring at a temperature of 45°C for 2 h. The high-speed shearing is controlled at a speed of 2000 r / min for 30 min. The spray drying is controlled at an inlet temperature of 160°C, an outlet temperature of 70°C, and a feeding speed of 5 mL / min. The washing is performed using anhydrous ethanol.
[0027] Example Two A water product feed preparation method based on the synergistic structure regulation of rare earth elements and α-starch comprises the following steps: Step 1, mixing: putting fish meal, soybean meal, mixed fillers, complex vitamins, and minerals into a mixer to mix and obtain a basic raw material mixture; Step 2, adding: sequentially adding rare earth-α-starch composite microcapsules, composite prebiotics, and oil to the basic raw material mixture, mixing and uniformly dispersing to obtain a functional mixture; Step 3, granulation: processing the functional mixture through an extruder to obtain feed particles; The mass fraction of fish meal, soybean meal, mixed fillers, complex vitamins, minerals, rare earth-α-starch composite microcapsules, composite prebiotics, and oil is 40:18:29:0.75:1:11.26:1:6.5.
[0028] The rare earth-α-starch composite microcapsule is obtained by amino modification and cross-linking coating of α-starch with rare earth complex. It should be noted that the α-starch is potato α-starch, and the molecular weight is 20-30 million Da. The rare earth complex is La(NO3)3·6H2O and Ce(NO3)3·6H2O with a mass ratio of 1:1.
[0029] The amino modification includes step ①: subjecting potato α-starch to low-temperature plasma treatment, and controlling the vacuum degree of the low-temperature plasma treatment to be 0.07 MPa, the power to be 100 W, and the treatment time to be 20 min, to obtain active starch under a mixed gas of Ar and oxygen with a volume ratio of 3:1; and step ②: mixing the active starch with 5% D-glucosamine hydrochloride solution according to a mass ratio of 1:4, controlling the pH to be 8.8, and stirring at a constant temperature of 56℃ for 2.5 h, and then filtering and drying to obtain amino-modified α-starch with a mass grafting rate of 10.31 wt%.
[0030] The cross-linking coating includes step ①: dissolving 0.04 parts of rare earth complex in deionized water to obtain a rare earth solution with a mass concentration of 6%, and then adding 0.4 parts of an active aid to the rare earth solution, stirring uniformly, and adjusting the pH to 5.8 to obtain a precursor solution; step ②: mixing 10 parts of amino-modified α-starch with deionized water according to a mass ratio of 1:3.5, controlling the temperature to be 62℃, and adding the precursor solution, to obtain an emulsion by high-speed shearing; step ③: adding 0.6 parts of a dynamic cross-linking agent to the emulsion, controlling the temperature to be 47℃, and stirring for 105 min to obtain a dynamic cross-linking coated starch solution; and step ④: adding 1 part of a plasticizer to the dynamic cross-linking coated starch solution, and then sequentially stirring, spray drying, and washing to obtain the finished rare earth-α-starch composite microcapsule.
[0031] In the cross-linking coating, the active aid is D-glucosamine hydrochloride, and the plasticizer is glycerol, both of which are commercially available and will not be described here. The dynamic cross-linking agent is chitosan-g-glutaraldehyde graft, which is obtained by adding 1 g of chitosan to 100 mL of 1% acetic acid aqueous solution according to a mass-volume ratio of 1 g:100 mL, controlling the temperature to be 50℃, stirring until completely dissolved, then adding 25% glutaraldehyde solution with a chitosan mass ratio of 10:1, controlling the pH to be 5.5, and stirring at a constant temperature of 45℃ for 2 h. The high-speed shearing is controlled at a speed of 2050 r / min for 29 min. The spray drying is controlled at an inlet air temperature of 165℃, an outlet air temperature of 75℃, and a feeding speed of 7 mL / min. The washing is performed with anhydrous ethanol.
[0032] Example Three A method for preparing aquatic feed based on the synergistic regulation of rare earth elements and α-starch structure, comprising the following steps: Step 1, mixing: the fish meal, soybean meal, mixed filler, compound vitamin, mineral are put into the mixer and stirred to obtain the base material mixture; Step 2, adding: the rare earth-α-starch composite microcapsule, compound prebiotic and oil are sequentially added to the base material mixture, and are mixed and dispersed uniformly to obtain a functional mixture; Step 3, granulation: the functional mixture is treated by an extruder to obtain feed particles; The mass ratio of the fish meal, soybean meal, mixed filler, compound vitamin, mineral, rare earth-α-starch composite microcapsule, compound prebiotic and oil is 42:19:32:0.9:1.8:12.245:1.2:7. The rare earth-α-starch composite microcapsule is obtained by amino modification and rare earth compound cross-linking coating of α-starch. It should be noted that the α-starch is potato α-starch, and the molecular weight is 20-30 million Da. The rare earth compound is La(NO3)3·6H2O and Ce(NO3)3·6H2O with a mass ratio of 1:1.05.
[0033] The amino modification includes step ①: the potato α-starch is subjected to low temperature plasma treatment, and the vacuum degree of the low temperature plasma treatment is controlled to be 0.08 MPa, the power is 120 W, and the treatment time is 15 min, and the active starch is obtained under the mixed gas of Ar and oxygen with a volume ratio of 3:1; step ②: the active starch is mixed with 5% D-glucosamine hydrochloride solution according to a mass ratio of 1:4.2, and the pH is controlled to be 9.0, the temperature is controlled to be 60°C, and the stirring is controlled for 3 h, and then the amino-modified α-starch with a mass grafting rate of 11.75wt% is obtained after filtration and drying.
[0034] The cross-linking coating includes step ①: 0.045 parts of the rare earth compound is dissolved in deionized water to obtain a rare earth solution with a mass concentration of 6%, and then 0.5 parts of an active aid is added to the rare earth solution, stirred uniformly, and the pH is adjusted to 6.0 to obtain a precursor solution; step ②: 11 parts of the amino-modified α-starch is mixed with deionized water according to a mass ratio of 1:3.6, the temperature is controlled to be 65°C, and the precursor solution is added, and an emulsion is obtained by high-speed shearing; step ③: 0.7 parts of a dynamic cross-linking agent is added to the emulsion, the temperature is controlled to be 50°C, and the stirring treatment is controlled for 90 min to obtain a dynamic cross-linking coated starch solution; step ④: 1.05 parts of a plasticizer is added to the dynamic cross-linking coated starch solution, and then the stirring, spray drying and washing are sequentially performed to obtain the finished product of the rare earth-α-starch composite microcapsule.
[0035] The active assistant used in the cross-linking coating is D-glucosamine hydrochloride, and the plasticizer is glycerol, both of which are commercially available and will not be described here. The dynamic cross-linking agent is chitosan-g-glutaraldehyde graft, which is obtained by adding chitosan with a mass-volume ratio of 1 g:100 mL into 1% acetic acid aqueous solution, controlling the temperature to be 50°C and stirring until completely dissolved, then adding 25% glutaraldehyde solution with a mass ratio of 10:1 to chitosan, controlling the pH to be 6.0, and stirring at a constant temperature of 45°C for 2 h. The high-speed shearing is controlled at a speed of 2100 r / min for 30 min. The spray drying is controlled at an inlet temperature of 170°C, an outlet temperature of 80°C, and a feeding speed of 8 mL / min. The washing is performed using anhydrous ethanol.
[0036] Comparative Example One The difference between Comparative Example One and Example Three is that the α-starch in Comparative Example One is not subjected to amino modification.
[0037] Comparative Example Two The difference between Comparative Example Two and Example Three is that the rare earth-α-starch composite microcapsule in Comparative Example Two is replaced by 0.045 parts of rare earth composite and 11 parts of α-starch subjected to amino modification.
[0038] Comparative Example Three The difference between Comparative Example Three and Example Three is that the cross-linking coating in Comparative Example Three does not have step ④.
[0039] Comparative Example Four The difference between Comparative Example Four and Example Three is that the dynamic cross-linking agent in Comparative Example Four is citric acid, which is commercially available.
[0040] Performance Test: 1. In vitro slow-release performance test: Simulate the gastrointestinal environment according to “GB / T 23527-2009 Determination of acidity in feed”, incubate the feed sample in the stomach environment (pH 2.5, 37°C, 2h) and the intestinal environment (pH 7.0, 37°C, 12h) respectively, determine the rare earth content in the release liquid, and calculate the cumulative release rate; 2. Growth performance test: Select healthy eels with an initial body weight of (50±5) g, 3 replicates per group, 30 eels per replicate, and a cultivation period of 12 weeks, according to “SC / T 1077-2004 Eel compound feed”, determine the weight gain rate = (final body weight-initial body weight) / initial body weight x 100%, and the feed coefficient = total food intake / total weight gain; 3. Safety test: According to GB 13078-2017 Feed Hygiene Standard, the rare earth residue (ICP-MS method) and heavy metal (lead, cadmium) content in the finished feed were determined; after the breeding was completed, the rare earth residue in the muscle of eel was determined; 4. Heat stability test: Using a thermal gravimetric analyzer (TGA), under a nitrogen atmosphere, the temperature at which the mass loss of the microcapsule was 5% was recorded at a heating rate of 10℃ / min from room temperature to 300℃.
[0041] Performance tests were performed on the above embodiment one to embodiment three and comparative example one to comparative example three, and the performance test results are shown in Table 1.
[0042] Table 1 Performance test results
[0043] From the above Table 1, it can be seen that the growth performance in the third embodiment of the present application is the highest, reaching 216.1%, and the safety all meets less than 0.5mg / kg, which meets the GB 13078-2017 standard, and the heat stability in the first embodiment to the third embodiment is all greater than 225℃, it can be seen that the synergistic scheme of plasma amino modification and chitosan-g-glutaraldehyde dynamic cross-linking will form a dense and stable network composite structure, so as to effectively resist high temperature processing while reducing the loss of rare earth. The in vitro slow-release performance of comparative example one and comparative example two is less than 65%. It can be seen that when there is no effective cross-linking coating, the rare earth will be easily released or lost in the stomach environment in advance, and since comparative example four uses citric acid, it will cause the cross-linking network structure formed to have a too fast degradation rate, thereby causing the slow-release period to be shortened.
[0044] In summary, the present application provides a water product feed preparation method based on rare earth element synergistic α-starch structure regulation. The water product feed preparation method based on rare earth element synergistic α-starch structure regulation introduces active groups through plasma activation, and constructs a double combination through synergistic dynamic Schiff base cross-linking, realizes the physical embedding and chemical coordination synergistic effect of rare earth and α-starch, improves the processing stability of the water product feed based on rare earth element synergistic α-starch structure regulation and achieves the purpose of intestinal targeted slow release, realizes the effect of significantly improving the digestion and absorption and growth performance of aquatic animals, improving intestinal health, and reducing nitrogen and phosphorus emissions and antibiotic dependence.
[0045] The use of "first", "second", "third", "fourth" etc. (if any) in this disclosure is only to distinguish similar objects, and does not necessarily indicate a particular order or sequence. It should be understood that the data thus used can be interchanged under appropriate circumstances, so that the embodiments described herein can be implemented in an order other than that described herein. In addition, the terms "comprise" and "have" and any variations thereof are intended to cover non-exclusive inclusion, for example, a process, method or device comprising a series of steps or units does not necessarily limit to those clearly listed steps or units, but can include other steps or units not clearly listed or inherent to these processes, methods or devices.
[0046] It should be noted that the description involving "first", "second" etc. in this application is only for the purpose of description, and cannot be understood as indicating or implying the relative importance of the indicated technical features or implicitly indicating the number of the indicated technical features. Therefore, the features defined with "first", "second" can explicitly or implicitly include at least one of the features. In addition, the technical solutions of various embodiments can be combined with each other, but it must be based on the realization of ordinary skilled in the art, when the combination of technical solutions appears contradictory or unachievable, it should be considered that the combination of technical solutions does not exist, nor within the scope of protection claimed in this application.
[0047] The principles and implementation modes of the present application are described by applying specific examples herein, and the above description of the examples is only for the purpose of helping to understand the method of the present application and its core idea; at the same time, for those skilled in the art, according to the idea of the present application, the specific implementation mode and application range will be changed, and the above description of the specification should not be understood as limiting the present application.
Claims
1. A method for preparing aquatic feed based on synergistic regulation of rare earth elements and α-starch structure, characterized in that, It comprises the following steps: Step 1, mixing: the fish meal, soybean meal, mixed filler, compound vitamin, mineral are put into the mixer for stirring and mixing to obtain a basic raw material mixture; Step 2, adding: the rare earth-α-starch composite microcapsule, compound prebiotic and oil are sequentially added into the basic raw material mixture, which is mixed and dispersed uniformly to obtain a functional mixture; Step 3, granulation: the functional mixture is treated by an extruder to obtain feed particles; The mass ratio of the fish meal, soybean meal, mixed filler, compound vitamin, mineral, rare earth-α-starch composite microcapsule, compound prebiotic and oil is 38-42：16-19:26-32:0.6-0.9:1.2-1.8:9.73-12.245:0.8-1.2:6-7； The rare earth-α-starch composite microcapsule is obtained by coating the α-starch with amino modification and rare earth compound crosslinking.
2. The method for preparing aquatic feed based on synergistic regulation of rare earth elements and α-starch structure according to claim 1, characterized in that: The α-starch is potato α-starch, and the molecular weight is 20-300 million Da, and the amino modification comprises the following steps: ① the potato α-starch is subjected to low temperature plasma treatment, and the vacuum degree of the low temperature plasma treatment is controlled to be 0.05-0.08 MPa, the power is 80-120 W, and the treatment time is 15-25 min, and the active starch is obtained under the mixed gas of Ar and oxygen with a volume ratio of 3:1; ② the active starch is mixed with 5% D-glucosamine hydrochloride solution according to the mass ratio of 1:3.8-4.2, and the pH is controlled to be 8.5-9.0, and the temperature is controlled to be 55-60℃, and the stirring is carried out for 2-3 h, and then the amino α-starch with a mass grafting rate of 8-12wt% is obtained after filtration and drying.
3. The method according to claim 1, characterized in that: The rare earth compound is La(NO3)3·6H2O and Ce(NO3)3·6H2O with a mass ratio of 1:0.9-1.
05.
4. The method according to claim 3, characterized in that: The crosslinking coating comprises the following steps: ① 0.03-0.045 parts of the rare earth compound is dissolved in deionized water to obtain a rare earth solution with a mass concentration of 6%, and then 0.3-0.5 parts of an active aid is added to the rare earth solution, and after stirring uniformly, the pH is adjusted to 5.5-6.0 to obtain a precursor solution; ② 9-11 parts of the α-starch modified by amino is mixed with deionized water according to the mass ratio of 1:3.3-3.6, the temperature is controlled to be 60-65℃, and the precursor solution is added, and an emulsion is obtained by high-speed shearing; ③ 0.4-0.7 parts of a dynamic crosslinking agent is added to the emulsion, the temperature is controlled to be 45-50℃, and stirring treatment is carried out for 90-120 min to obtain a dynamic crosslinking coated starch solution; ④ 0.95-1.05 parts of a plasticizer is added to the dynamic crosslinking coated starch solution, and after stirring, spray drying and washing in sequence, the finished product of the rare earth-α-starch composite microcapsule is obtained.
5. The method for preparing aquatic feed based on synergistic regulation of rare earth elements and α-starch structure according to claim 4, characterized in that: The active aid is D-glucosamine hydrochloride, the dynamic crosslinking agent is chitosan-g-glutaraldehyde graft, and the plasticizer is glycerol.
6. The method for preparing aquatic feed based on synergistic regulation of rare earth elements and α-starch structure according to claim 4, characterized in that: The high-speed shearing is controlled at a speed of 2000-2100 r / min for 28-30 min.
7. The method according to claim 4, characterized in that: The spray drying is controlled with an air inlet temperature of 160-170 DEG C, an air outlet temperature of 70-80 DEG C, and a feeding speed of 5-8 mL / min; the washing is carried out with anhydrous ethanol; the particle size of the rare earth-alpha-starch composite microcapsule is 8-15 mu m, the embedding rate is greater than or equal to 95%, and the coordination combination rate is greater than or equal to 75%.
8. The method for preparing aquatic feed based on synergistic regulation of rare earth elements and α-starch structure according to claim 1, characterized in that: The mixed filling is bran and oat powder at a mass ratio of 2-2.2:1; the composite vitamin is VA / VD / VE composite vitamin; and the mineral is calcium / phosphorus / zinc composite mineral.
9. The method according to claim 1, characterized in that: The composite prebiotic is fructo-oligosaccharide and inulin at a mass ratio of 1:0.95-1.
10. The method for preparing aquatic feed based on synergistic regulation of rare earth elements and α-starch structure according to claim 1, characterized in that: The oil and fat is fish oil and / or bean oil.