Deep sea fish oil type micro-capsule milk fat powder feed and preparation method thereof

Abstract

The invention relates to the technical field of feeds, in particular to a deep sea fish oil type micro-capsule milk fat powder feed and a preparation method thereof, and the deep sea fish oil type micro-capsule milk fat powder feed comprises the following raw materials in parts by weight: 35-38 parts of fish meal, 20-25 parts of soybean meal, 10-12 parts of compound fish oil microcapsules, 3-5 parts of corn protein powder, 1-1.2 parts of monocalcium phosphate, 0.3-0.5 part of soybean phosphate and 0.08-0.1 part of an antioxidant; the compound fish oil microcapsule added into the feed forms an anti-oxidation system from inside to outside through a microcapsule wall material cyclodextrin inclusion compound, oxidation rancidity of deep sea fish oil is avoided to the greatest extent, and due to double crosslinking of zinc acetate and sodium polyphosphate, a formed compact shell ensures the stability of the deep sea fish oil in the processing and storage processes, so that the deep sea fish oil is prevented from being oxidized and rancidified. And animal food refusal behaviors caused by fishy smell of the deep sea fish oil are reduced.

Description

TECHNICAL FIELD

[0001] The present application relates to the technical field of feed, in particular to a deep-sea fish oil type microcapsule milk fat powder feed and a preparation method thereof. BACKGROUND

[0002] Deep-sea fish oil is rich in long-chain polyunsaturated fatty acids such as eicosapentaenoic acid and docosahexaenoic acid, which is of great significance to promote animal growth and development, improve body health, and improve the quality of livestock and aquatic products. However, the highly unsaturated nature of deep-sea fish oil makes it prone to oxidation and spoilage during processing, storage and transportation, resulting in loss of nutritional value, production of harmful substances, and generation of fishy odor, which seriously restricts its large-scale application in feed. For example, patent CN105558354A “Feed fish oil microcapsule and its preparation process” uses a double-layer structure microcapsule technology to protect fish oil, delay fish oil oxidation, and mask fishy odor. However, it still has problems of insufficient mechanical strength and stability in complex feed environment, and it cannot reduce fish oil oxidation caused by the environment, so a fish oil microcapsule with strong oxidation stability and tolerance to feed processing conditions is needed, and a milk fat powder feed with the fish oil microcapsule as an additive is needed. SUMMARY

[0003] The purpose of the present application is to provide a deep-sea fish oil type microcapsule milk fat powder feed and a preparation method thereof. The composite fish oil microcapsule added in the feed is formed by cyclodextrin inclusion in the microcapsule shell material to form an antioxidant system from the inside out, which maximizes the prevention of deep-sea fish oil oxidation and spoilage. The dense shell formed by the double crosslinking of zinc acetate and sodium polyphosphate ensures the stability of the microcapsule during processing and storage, and reduces the animal's refusal to eat caused by the fishy odor of deep-sea fish oil.

[0004] The purpose of the present application can be achieved by the following technical solution: a preparation method of a deep-sea fish oil type microcapsule milk fat powder feed, comprising the following steps: weighing the following raw materials: 35-38 parts of fish meal, 20-25 parts of soybean meal, 10-12 parts of composite fish oil microcapsule, 3-5 parts of corn gluten meal, 1-1.2 parts of calcium dihydrogen phosphate, 0.3-0.5 parts of soybean phosphate, and 0.08-0.1 parts of antioxidant. Mix the fish meal, soybean meal, composite fish oil microcapsule, corn gluten meal, calcium dihydrogen phosphate, soybean phosphate and antioxidant to obtain a deep-sea fish oil type microcapsule milk fat powder feed.

[0005] The composite fish oil microcapsule is prepared by the following steps: Step A1: chitosan and ethanol were mixed, stirred at a stirring rate of 100-120 rpm and room temperature for 30-40 min, then vanillin was added, and the temperature was raised to 60℃, and stirred for 12-15 min, then glacial acetic acid was added, and reacted for 10-12 h, and then chitosan Schiff base was prepared by rotary evaporation and washing; Further, in step A1: the amount ratio of chitosan, ethanol, vanillin and glacial acetic acid was 0.5-0.6 g: 45-50 mL: 0.82-0.85 g: 3-4 mL.

[0006] Step A2: chitosan Schiff base and glacial acetic acid solution were mixed, stirred at a stirring rate of 100-120 rpm and 35℃ for 3-4 h, then cyclodextrin inclusion compound was added, and stirred for 3-4 h, then the water phase was prepared, deep sea fish oil and Tween-80 were mixed to prepare the oil phase, and then the oil phase was added to the water phase under stirring at a stirring rate of 7000-8000 rpm and room temperature, and emulsified for 8-10 min to prepare the emulsion; Further, in step A2: the amount ratio of chitosan Schiff base, glacial acetic acid solution, cyclodextrin inclusion compound, deep sea fish oil and Tween-80 was 1-1.2 g: 90-100 mL: 0.45-0.5 g: 2.2-2.5 mL: 0.18-0.2 g.

[0007] Step A3: sodium hydroxide solution was added to the emulsion to adjust the pH value to 5.5, then zinc acetate aqueous solution was added, and reacted for 25-30 min at a stirring rate of 350-400 rpm and 55℃, then sodium polyphosphate solution was added, and reacted for another 25-30 min, then sodium hydroxide solution was added again to adjust the pH value to 7, and then the composite fish oil microcapsule was prepared by spray drying; Further, in step A3: the amount ratio of emulsion, zinc acetate aqueous solution and sodium polyphosphate solution was 85-90 mL: 3.8-4 mL: 4.5-5 mL, the mass fraction of sodium hydroxide solution was 3%, the mass fraction of zinc acetate aqueous solution was 5%, and the mass fraction of sodium polyphosphate solution was 3%.

[0008] Further, in the reaction process, the Schiff base structure was formed by the reaction of amino group in chitosan and aldehyde group in vanillin to prepare chitosan Schiff base, and then the composite fish oil microcapsule was prepared by the emulsion method, with chitosan Schiff base as the main wall material, zinc acetate and sodium polyphosphate as the complexing cross-linking agent, and cyclodextrin inclusion compound as the wall material dopant, and by spray drying technology.

[0009] The cyclodextrin inclusion compound was prepared by the following steps: Step B1: mix beta-cyclodextrin and deionized water, stir and add sodium hydroxide solution, adjust pH value to 8.5, stir at a stirring rate of 100-120 rpm and a temperature of 50 DEG C, and then add octadecyl succinic anhydride, react for 3.5-4 h, add hydrochloric acid solution to adjust pH value to 6.5, freeze-dry, wash, and obtain the amphiphilic cyclodextrin; Further, in step B1, the ratio of beta-cyclodextrin, deionized water and octadecyl succinic anhydride is 9.8-10 g:100-110 mL:5.6-5.8 g, the mass fraction of sodium hydroxide solution is 2%, and the mass fraction of hydrochloric acid solution is 2%.

[0010] Step B2: mix the amphiphilic cyclodextrin and deionized water, stir at a stirring rate of 100-120 rpm and a temperature of 50 DEG C for 15-20 min, cool to 40 DEG C, and then add tea polyphenol, ultrasonic dispersion for 8-10 min, continue to stir for 2.5-3 h, stand for 10-12 h at a temperature of 15 DEG C, centrifugal, wash, freeze-dry, and obtain the cyclodextrin inclusion compound. Further, in step B2, the ratio of the amphiphilic cyclodextrin, deionized water and tea polyphenol is 11.8-12 g:100-110 mL:2-2.1 g.

[0011] Further, in the reaction process, the beta-cyclodextrin is used as raw material, the ester group is formed by the reaction of the hydroxyl group in the beta-cyclodextrin and the acid anhydride in the octadecyl succinic anhydride under alkaline conditions, the amphiphilic cyclodextrin is obtained, and due to the special structure of the hydrophilic outer side and the hydrophobic inner cavity of the amphiphilic cyclodextrin and the introduction of the hydrophobic alkyl long chain by graft modification, the tea polyphenol is added and ultrasonic dispersion is carried out, and since the tea polyphenol has hydrophilic and hydrophobic parts, it can be embedded into the inner cavity of the amphiphilic cyclodextrin, thereby forming the host-guest structure, and the hydrogen bond is formed with the inner cavity of the cyclodextrin, and the cyclodextrin inclusion compound is obtained.

[0012] The present application has the following beneficial effects: the present application discloses a kind of deep sea fish oil type microcapsule cream powder feed and preparation method thereof, and the compound fish oil microcapsule added in feed is formed from inside to outside antioxidant system by microcapsule shell material cyclodextrin inclusion compound, which avoids the oxidation of deep sea fish oil to the greatest extent, and the dense shell formed by double crosslinking ensures the stability in processing and storage, and reduces the animal refusal behavior caused by the fishy smell of deep sea fish oil.

[0013] The prepared composite fish oil microcapsule has the tea polyphenol-encapsulated β-cyclodextrin introduced into the wall material, and the formed cyclodextrin inclusion compound has amphiphilicity, which can not only encapsulate tea polyphenol, but also can be used as the wall material doped in the microcapsule forming process, so that the cyclodextrin inclusion compound can play an antioxidant effect from inside to outside to reduce the antioxidant performance of the sound contained in the microcapsule core material; and since the main material of the wall material is chitosan Schiff base, the zinc acetate and sodium polyphosphate are added in sequence, and both of them can be coordinated with the chitosan Schiff base to form a double crosslinking system, so that the microcapsule shell layer is more dense, and the stability in the storage process is improved, and the dense shell layer can greatly improve the odor shielding effect, reduce the animal's refusal behavior caused by the fishy smell of deep sea fish oil, and the zinc and phosphorus elements contained therein can also be used as the source of trace elements in feed. DETAILED DESCRIPTION

[0014] The technical solutions in the embodiments of the present application will be described clearly and completely below. Obviously, the described embodiments are only part of the embodiments of the present application, rather than all the embodiments. Based on the embodiments in the present application, all other embodiments obtained by those skilled in the art without creative labor fall within the protection scope of the present application.

[0015] Example 1: A preparation method of a deep sea fish oil type microcapsule milk fat powder feed, comprising the following steps: weighing the following weight parts of raw materials: 35 parts of fish meal, 20 parts of soybean meal, 10 parts of composite fish oil microcapsule, 3 parts of corn gluten meal, 1 part of calcium dihydrogen phosphate, 0.3 parts of soybean phosphate, and 0.08 parts of antioxidant, and mixing the fish meal, soybean meal, composite fish oil microcapsule, wheat meal, corn gluten meal, calcium dihydrogen phosphate, soybean phosphate and antioxidant to prepare a deep sea fish oil type microcapsule milk fat powder feed.

[0016] Further, the fish meal is from Shandong Ken Sheng Chemical Co., Ltd., and the model is TASA; the soybean meal is from Beijing Jiahe Mofeng Feed Co., Ltd., and the model is RW30; the corn gluten meal is from Wudi Zhaoxin Feed Co., Ltd., and the model is ZX005; and the antioxidant is from Hebei Jiuxing Chemical Product Co., Ltd., and the model is BHT.

[0017] The composite fish oil microcapsule is prepared by the following steps: Step A1: chitosan and ethanol are mixed, stirred at a stirring rate of 100 rpm and room temperature for 30 min, then vanillin is added, and the temperature is increased to 60℃, and the stirring is continued for 12 min, then glacial acetic acid is added, and the reaction is carried out for 10 h, then rotary evaporation is carried out, and washing is carried out to prepare chitosan Schiff base; Further, in step A1: the amount ratio of chitosan, ethanol, vanillin and glacial acetic acid is 0.5g:45mL:0.82g:3mL; Further, the chitosan is from Shanghai Aladdin Biochem Technology Co., Ltd., model C434547.

[0018] Step A2: mix the chitosan Schiff base and glacial acetic acid solution, stir at a stirring rate of 100rpm and a temperature of 35℃ for 3h, then add the cyclodextrin inclusion compound, continue to stir for 3h, prepare the water phase, mix the deep sea fish oil and Tween-80, prepare the oil phase, under the condition of stirring rate of 7000rpm and room temperature, add the oil phase into the water phase, emulsify for 8min, prepare the emulsion; Further, in step A2: the amount ratio of chitosan Schiff base, glacial acetic acid solution, cyclodextrin inclusion compound, deep sea fish oil and Tween-80 is 1g:90mL:0.45g:2.2mL:0.18g.

[0019] Step A3: add sodium hydroxide solution into the emulsion, adjust the pH value to 5.5, stir and add zinc acetate aqueous solution, under the condition of stirring rate of 350rpm and temperature of 55℃, react for 25min, then add sodium polyphosphate solution, continue to react for 25min, add sodium hydroxide solution again, adjust the pH value to 7, spray dry, prepare the composite fish oil microcapsule; Further, in step A3: the amount ratio of emulsion, zinc acetate aqueous solution and sodium polyphosphate solution is 85mL:3.8mL:4.5mL, the mass fraction of sodium hydroxide solution is 3%, the mass fraction of zinc acetate aqueous solution is 5%, and the mass fraction of sodium polyphosphate solution is 3%; Further, the sodium polyphosphate is from Shanghai Aladdin Biochem Technology Co., Ltd., model S165313.

[0020] The cyclodextrin inclusion compound is prepared by the following steps: Step B1: mix β-cyclodextrin and deionized water, stir and add sodium hydroxide solution, adjust the pH value to 8.5, under the condition of stirring rate of 120rpm and temperature of 50℃, stir and add octadecyl succinic anhydride, react for 3.5h, then add hydrochloric acid solution to adjust the pH value to 6.5, freeze-dry, wash, prepare the amphiphilic cyclodextrin; Further, in step B1: the amount ratio of β-cyclodextrin, deionized water and octadecyl succinic anhydride is 9.8g:110mL:5.6g, the mass fraction of sodium hydroxide solution is 2%, and the mass fraction of hydrochloric acid solution is 2%.

[0021] Step B2: Mix the amphiphilic cyclodextrin and deionized water, stir for 20 min at a stirring rate of 100 rpm and a temperature of 50℃, cool to 40℃, and add tea polyphenols, ultrasonic dispersion for 8 min, continue to stir for 2.5 h, and then stand for 12 h at a temperature of 15℃, centrifugal, washing, freeze-drying, to prepare cyclodextrin inclusion compound; Further, in step B2: the dosage ratio of amphiphilic cyclodextrin, deionized water and tea polyphenol is 12g:110mL:2g; Further, the tea polyphenol is from Shanghai Aladdin Biochem Technology Co., Ltd., model T418534.

[0022] Example 2 A preparation method of a deep sea fish oil type microcapsule milk fat powder feed, comprising the following steps: weighing the following weight parts of raw materials: 38 parts of fish meal, 20 parts of soybean meal, 10 parts of compound fish oil microcapsule, 3 parts of corn gluten meal, 1.2 parts of calcium dihydrogen phosphate, 0.3 parts of soybean phosphate and 0.1 parts of antioxidant, mixing the fish meal, soybean meal, compound fish oil microcapsule, wheat flour, corn gluten meal, calcium dihydrogen phosphate, soybean phosphate and antioxidant to prepare a deep sea fish oil type microcapsule milk fat powder feed.

[0023] Further, the fish meal is from Shandong Ken Sheng Chemical Co., Ltd., model TASA; the soybean meal is from Beijing Jiahuo Mufeng Feedstuff Co., Ltd., model RW30; the corn gluten meal is from Wudi Zhaoxin Feedstuff Co., Ltd., model ZX005; and the antioxidant is from Hebei Jiuxing Chemical Products Co., Ltd., model BHT.

[0024] The compound fish oil microcapsule is prepared by the following steps: Step A1: Mix chitosan and ethanol, stir for 40 min at a stirring rate of 100 rpm and a temperature of room temperature, then add vanillin and heat to 60℃, continue to stir for 15 min, stir and add glacial acetic acid, react for 10 h, rotary evaporation, washing, to prepare chitosan Schiff base; Further, in step A1: the dosage ratio of chitosan, ethanol, vanillin and glacial acetic acid is 0.5g:45mL:0.85g:3mL; Further, the chitosan is from Shanghai Aladdin Biochem Technology Co., Ltd., model C434547.

[0025] Step A2: Mix the chitosan Schiff base and glacial acetic acid solution, stir for 4 h at a stirring rate of 120 rpm and a temperature of 35℃, then add cyclodextrin inclusion compound, continue to stir for 4 h, to prepare an aqueous phase, mix deep sea fish oil and Tween-80 to prepare an oil phase, emulsify the oil phase into the aqueous phase at a stirring rate of 7000 rpm and room temperature for 8 min to prepare an emulsion; Further, in step A2: the dosage ratio of chitosan Schiff base, glacial acetic acid solution, cyclodextrin inclusion compound, deep-sea fish oil and Tween-80 is 1g:90mL:0.5g:2.2mL:0.2g.

[0026] Step A3: add sodium hydroxide solution to the emulsion to adjust the pH value to 5.5, stir and add zinc acetate aqueous solution, under the condition of stirring rate of 350rpm and temperature of 55℃, react for 30min, then add sodium polyphosphate solution, continue to react for 25min, add sodium hydroxide solution again to adjust the pH value to 7, and spray dry to obtain the composite fish oil microcapsule; Further, in step A3: the dosage ratio of emulsion, zinc acetate aqueous solution and sodium polyphosphate solution is 85mL:4mL:4.5mL, the mass fraction of sodium hydroxide solution is 3%, the mass fraction of zinc acetate aqueous solution is 5%, and the mass fraction of sodium polyphosphate solution is 3%; Further, the sodium polyphosphate is from Shanghai Aladdin Biochem Technology Co., Ltd., model S165313.

[0027] The cyclodextrin inclusion compound is prepared by the following steps: Step B1: mix β-cyclodextrin and deionized water, stir and add sodium hydroxide solution to adjust the pH value to 8.5, under the condition of stirring rate of 100rpm and temperature of 50℃, stir and add octadecyl succinic anhydride, react for 3.5h, then add hydrochloric acid solution to adjust the pH value to 6.5, freeze-dry, wash and obtain the amphiphilic cyclodextrin; Further, in step B1: the dosage ratio of β-cyclodextrin, deionized water and octadecyl succinic anhydride is 9.8g:100mL:5.6g, the mass fraction of sodium hydroxide solution is 2%, and the mass fraction of hydrochloric acid solution is 2%.

[0028] Step B2: mix the amphiphilic cyclodextrin and deionized water, under the condition of stirring rate of 100rpm and temperature of 50℃, stir for 15min, cool to 40℃ and add tea polyphenol, ultrasonic dispersion for 8min, continue to stir for 2.5h, then stand for 10h at temperature of 15℃, centrifuge, wash, freeze-dry and obtain the cyclodextrin inclusion compound; Further, in step B2: the dosage ratio of amphiphilic cyclodextrin, deionized water and tea polyphenol is 11.8g:100mL:2g; Further, the tea polyphenol is from Shanghai Aladdin Biochem Technology Co., Ltd., model T418534.

[0029] A preparation method of a deep-sea fish oil type microcapsule milk fat powder feed, comprising the following steps: weighing the following raw materials: 38 parts of fish meal, 25 parts of soybean meal, 12 parts of compound fish oil microcapsule, 5 parts of corn gluten meal, 1.2 parts of calcium dihydrogen phosphate, 0.5 parts of soybean phosphate, and 0.1 parts of antioxidant, mixing the fish meal, soybean meal, compound fish oil microcapsule, wheat flour, corn gluten meal, calcium dihydrogen phosphate, soybean phosphate and antioxidant to prepare a deep-sea fish oil type microcapsule milk fat powder feed.

[0030] Further, the fish meal is from Shandong Ken Sheng Chemical Co., Ltd., model TASA; the soybean meal is from Beijing Jiahe Mofeng Feedstuff Co., Ltd., model RW30; the corn gluten meal is from Wudi Zhaoxin Feedstuff Co., Ltd., model ZX005; and the antioxidant is from Hebei Jiuxing Chemical Product Co., Ltd., model BHT.

[0031] The compound fish oil microcapsule is prepared by the following steps: Step A1: mixing chitosan and ethanol, stirring at a stirring rate of 120 rpm and room temperature for 40 min, then adding vanillin and heating to 60℃, continuing to stir for 15 min, stirring and adding glacial acetic acid, reacting for 12 h, rotary evaporation, washing, to prepare chitosan Schiff base; Further, in step A1: the amount ratio of chitosan, ethanol, vanillin and glacial acetic acid is 0.6 g: 50 mL: 0.85 g: 4 mL; Further, the chitosan is from Shanghai Aladdin Biochem Technology Co., Ltd., model C434547.

[0032] Step A2: mixing chitosan Schiff base and glacial acetic acid solution, stirring at a stirring rate of 120 rpm and 35℃ for 4 h, then adding cyclodextrin inclusion compound, continuing to stir for 4 h, to prepare water phase, mixing deep-sea fish oil and Tween-80 to prepare oil phase, emulsifying at a stirring rate of 8000 rpm and room temperature for 10 min to prepare emulsion; Further, in step A2: the amount ratio of chitosan Schiff base, glacial acetic acid solution, cyclodextrin inclusion compound, deep-sea fish oil and Tween-80 is 1.2 g: 100 mL: 0.5 g: 2.5 mL: 0.2 g.

[0033] Step A3: adding sodium hydroxide solution in the emulsion to adjust the pH value to 5.5, stirring and adding zinc acetate aqueous solution, reacting at a stirring rate of 400 rpm and 55℃ for 30 min, then adding sodium polyphosphate solution, continuing to react for 30 min, again adding sodium hydroxide solution to adjust the pH value to 7, and spray drying to prepare compound fish oil microcapsule; Further, in step A3: the ratio of the amount of emulsion, zinc acetate aqueous solution, and sodium polyphosphate solution is 90 mL:4 mL:5 mL, the mass fraction of sodium hydroxide solution is 3%, the mass fraction of zinc acetate aqueous solution is 5%, and the mass fraction of sodium polyphosphate solution is 3%; Further, the sodium polyphosphate is from Shanghai Aladdin Biochem Technology Co., Ltd., and the model number is S165313.

[0034] The cyclodextrin inclusion compound is prepared by the following steps: Step B1: β-cyclodextrin and deionized water are mixed, stirring is performed, and sodium hydroxide solution is added to adjust the pH value to 8.5. Stirring is performed at a stirring rate of 120 rpm and a temperature of 50°C, and stearic acid anhydride is added. Reaction is performed for 4 h, hydrochloric acid solution is added to adjust the pH value to 6.5, freeze-drying is performed, and washing is performed to prepare amphiphilic cyclodextrin. Further, in step B1: the ratio of the amount of β-cyclodextrin, deionized water, and stearic acid anhydride is 10 g:110 mL:5.8 g, the mass fraction of sodium hydroxide solution is 2%, and the mass fraction of hydrochloric acid solution is 2%.

[0035] Step B2: amphiphilic cyclodextrin and deionized water are mixed, stirring is performed at a stirring rate of 120 rpm and a temperature of 50°C for 20 min, the temperature is lowered to 40°C, and tea polyphenol is added. Ultrasonic dispersion is performed for 10 min, stirring is continuously performed for 3 h, the temperature is lowered to 15°C, and standing is performed for 12 h. Centrifugation is performed, washing is performed, freeze-drying is performed, and cyclodextrin inclusion compound is prepared. Further, in step B2: the ratio of the amount of amphiphilic cyclodextrin, deionized water, and tea polyphenol is 12 g:110 mL:2.1 g. Further, the tea polyphenol is from Shanghai Aladdin Biochem Technology Co., Ltd., and the model number is T418534.

[0036] Comparative Example 1: Compared with Example 3, the cyclodextrin inclusion compound in the preparation process of the fish oil microcapsule in Example 3 is replaced with the amphiphilic cyclodextrin in Example 3, and other steps are the same.

[0037] Comparative Example 2: Compared with Example 3, the zinc acetate aqueous solution in the preparation process of the fish oil microcapsule in Example 3 is removed, and other steps are the same.

[0038] The composite fish oil microcapsules prepared in Example 1, Example 2, Example 3, Comparative Example 1 and Comparative Example 2 were measured for surface oil content according to SC / T 3505-2006, and the results were recorded. 2 g of the composite fish oil microcapsules were added to a 37 wt% hydrochloric acid solution, and the mixture was incubated at 60°C for 30 min. The total oil content of the mixture was then measured by solvent extraction, and the results were recorded. The embedding rate was calculated as (total oil content-surface oil content) / total oil content*100%. The peroxide value of the composite fish oil microcapsules was measured according to SC / T 3505-2006, and the results were recorded. The prepared composite fish oil microcapsules were placed in an oven and incubated at 60°C for 7 d. The embedding rate and peroxide value of the composite fish oil microcapsules were then measured. The odor of the composite fish oil microcapsules after incubation was determined by sensory evaluation. The test results are shown in the following table:

[0039] As shown in the table, when Example 1, Example 2 and Example 3 were compared with Comparative Example 1 and Comparative Example 2, the results showed that, in Comparative Example 1, the cyclodextrin inclusion compound in the preparation process of the composite fish oil microcapsules of Example 3 was replaced by the amphiphilic cyclodextrin of Example 3. Due to the absence of tea polyphenol inclusion compound, the antioxidant effect was significantly reduced, and a certain fish oil odor appeared. In Comparative Example 2, the aqueous zinc acetate solution in the preparation process of the composite fish oil microcapsules of Example 3 was removed. Due to the absence of the double crosslinking structure, the wall material could not form a dense structure, and thus the embedding rate decreased rapidly after incubation, and the fish oil could not maintain good stability, and a significant fish oil rancidity odor appeared.

[0040] In the description of the specification, the description of the reference terms "one embodiment", "example", "specific example" and the like means that the specific features, structures, materials or characteristics described in connection with the embodiment or example are included in at least one embodiment or example of the present application. In the specification, the illustrative description of the above terms does not necessarily refer to the same embodiment or example. Moreover, the specific features, structures, materials or characteristics described can be combined in any one or more embodiments or examples in a suitable manner.

[0041] The above is only an example and description of the concept of the present application, and those skilled in the art can make various modifications or supplements to the described specific embodiments or use similar ways to replace them, as long as they do not deviate from the concept of the present application, which shall fall within the protection scope of the present application.

Claims

1. A process for the preparation of a deep sea fish oil type microencapsulated milk fat powder feedstuff, characterized in that: It comprises the following steps: weighing the following raw materials: 35-38 parts of fish meal, 20-25 parts of soybean meal, 10-12 parts of compound fish oil microcapsule, 3-5 parts of corn gluten meal, 1-1.2 parts of calcium dihydrogen phosphate, 0.3-0.5 parts of soybean phosphate and 0.08-0.1 parts of antioxidant, mixing fish meal, soybean meal, compound fish oil microcapsule, corn gluten meal, calcium dihydrogen phosphate, soybean phosphate and antioxidant to prepare a deep sea fish oil type microcapsule milk fat powder feed.

2. A process for the preparation of a deep sea fish oil type microencapsulated creamed powder feed as claimed in claim 1, wherein: The compound fish oil microcapsule is prepared by the following steps: Step A1: mixing chitosan and ethanol, stirring at a stirring rate of 100-120 rpm and room temperature for 30-40 min, then adding vanillin and heating to 60℃, continuing to stir for 12-15 min, stirring and adding glacial acetic acid, reacting for 10-12 h, rotary evaporation, washing to prepare chitosan Schiff base; Step A2: mixing chitosan Schiff base and glacial acetic acid solution, stirring at a stirring rate of 100-120 rpm and 35℃ for 3-4 h, then adding cyclodextrin inclusion compound, continuing to stir for 3-4 h to prepare water phase, mixing deep sea fish oil and Tween-80 to prepare oil phase, adding oil phase into water phase under stirring at a stirring rate of 7000-8000 rpm and room temperature, emulsifying for 8-10 min to prepare emulsion; Step A3: adding sodium hydroxide solution into emulsion to adjust pH value to 5.5, stirring and adding zinc acetate aqueous solution, reacting for 25-30 min at a stirring rate of 350-400 rpm and 55℃, then adding sodium polyphosphate solution, continuing to react for 25-30 min, adding sodium hydroxide solution again to adjust pH value to 7, spray drying to prepare compound fish oil microcapsule.

3. A process for the preparation of a deep sea fish oil type microencapsulated creamed powder feed as claimed in claim 2, characterized in that: In step A1: the amount ratio of chitosan, ethanol, vanillin and glacial acetic acid is 0.5-0.6 g: 45-50 mL: 0.82-0.85 g: 3-4 mL.

4. A process for the preparation of a deep sea fish oil type microencapsulated creamed powder feed as claimed in claim 2, wherein: In step A2: the amount ratio of chitosan Schiff base, glacial acetic acid solution, cyclodextrin inclusion compound, deep sea fish oil and Tween-80 is 1-1.2 g: 90-100 mL: 0.45-0.5 g: 2.2-2.5 mL: 0.18-0.2 g.

5. A process for the preparation of a deep sea fish oil type microencapsulated creamed powder feed as claimed in claim 2, wherein: In step A3: the amount ratio of emulsion, zinc acetate aqueous solution, sodium polyphosphate solution is 85-90 mL: 3.8-4 mL: 4.5-5 mL, the mass fraction of sodium hydroxide solution is 3%, the mass fraction of zinc acetate aqueous solution is 5%, and the mass fraction of sodium polyphosphate solution is 3%.

6. A process for the preparation of a deep sea fish oil type microencapsulated creamed powder feed as claimed in claim 2, wherein: The cyclodextrin inclusion compound is prepared by the following steps: Step B1: mixing β-cyclodextrin and deionized water, stirring and adding sodium hydroxide solution to adjust pH value to 8.5, stirring at a stirring rate of 100-120 rpm and 50℃, stirring and adding octadecyl succinic anhydride, reacting for 3.5-4 h, adding hydrochloric acid solution to adjust pH value to 6.5, freeze-drying, washing to prepare amphiphilic cyclodextrin; Step B2: Mix the amphiphilic cyclodextrin and deionized water, stir at a stirring rate of 100-120 rpm, at a temperature of 50℃ for 15-20 min, cool to 40℃, and add tea polyphenols, ultrasonic dispersion for 8-10 min, continue to stir for 2.5-3 h, and then stand at a temperature of 15℃ for 10-12 h, centrifuge, wash, freeze-dry, and obtain the cyclodextrin inclusion compound.

7. A process for the preparation of a deep sea fish oil type microencapsulated creamed powder feed according to claim 6, characterized in that: In step B1: the amount ratio of β-cyclodextrin, deionized water and octadecyl succinic anhydride is 9.8-10 g: 100-110 mL: 5.6-5.8 g, the mass fraction of sodium hydroxide solution is 2%, and the mass fraction of hydrochloric acid solution is 2%.

8. A process for the preparation of a deep sea fish oil type microencapsulated creamed powder feed as claimed in claim 6, characterized in that: In step B2: the amount ratio of amphiphilic cyclodextrin, deionized water and tea polyphenols is 11.8-12 g: 100-110 mL: 2-2.1 g.

9. A deep sea fish oil type microencapsulated milk fat powder feed characterized in that: Prepared according to the preparation method of any one of claims 1-8. Prepared according to the preparation method of any one of claims 1-8.

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