Quick-energy cream microcapsule and preparation method thereof

Abstract

The invention provides a quick-energy milk fat microcapsule and a preparation method thereof, and belongs to the technical field of microcapsules. Performing enzymolysis on deep sea fish oil, linseed oil and coconut oil, then adding the tea polyphenol / vitamin C fat-soluble substance to prepare a core material, adding the core material into an aqueous solution containing sodium alginate, konjac glucomannan and the carboxymethyl chitosan-whey protein condensate prepared in the step S4, and performing emulsification, centrifugation and freeze drying to prepare the quick-energy cream microcapsule. The prepared quick-energy milk fat microcapsule is uniform in size, small in size, easy to absorb and eat, good in mobility, long in shelf life and extremely easy to digest and absorb, can promote body health and growth and development of livestock, improves immunity, resists oxidation, inflammation, diseases and the like, and has a wide application prospect.

Description

Technical Field

[0001] The invention relates to the technical field of microcapsules, and in particular to a fast-energy milk fat microcapsule and a preparation method thereof. Background Art

[0002] Milk fat is one of the main components of milk. It contains many types of fatty acids, has high nutritional value, and has a specific aroma and soft texture. However, milk fat is not easy to dissolve, has a low melting point, is volatile, and is easily oxidized by oxygen, light, heat, heavy metals, etc., which limits the application of milk fat in food. Whey protein in milk is a high-quality complete protein with a reasonable composition of essential amino acids, high nutritional value, and easy digestion and absorption. It has good binding and good film-forming properties. It can be used alone or mixed with carbohydrates to make microcapsules of lipids, aromatic substances and flavor compounds. The preparation of whole milk component microcapsules with whey protein as the main wall material and milk fat as the core material is of great significance to expanding the application field and scope of milk components.

[0003] Milk fat microencapsulation is to encapsulate milk fat in closed spherical microcapsules of 5-200μm, which can not only prevent the oxidation of milk fat and the volatilization of flavor substances, but also make the milk fat into powder, which is more convenient for storage, transportation and use. The United States is the first country to carry out research on milk fat microcapsule preparation technology, and its main process is spray drying. The microcapsule milk fat prepared by spray drying has poor fluidity and short shelf life. Because it has to go through a high temperature process, it causes the loss and destruction of volatile substances and heat-sensitive flavor substances in milk fat and wall materials. Summary of the invention

[0004] The purpose of the present invention is to provide a fast-energy milk fat microcapsule and a preparation method thereof. The microcapsule is uniform in size, small in size, easy to absorb and eat, has good fluidity, long shelf life, is extremely easy to digest and absorb, can promote physical health, promote the growth and development of poultry and livestock, improve immunity, resist oxidation, inflammation, disease, etc., and has broad application prospects.

[0005] The technical solution of the present invention is achieved in this way:

[0006] The invention provides a method for preparing fast-energy milk fat microcapsules. The method comprises the following steps: enzymatically hydrolyzing deep-sea fish oil, linseed oil and coconut oil, adding tea polyphenols / vitamin C fat-soluble substances to obtain a core material, adding the core material to an aqueous solution containing sodium alginate, konjac glucomannan and the carboxymethyl chitosan-whey protein condensate obtained in step S4, emulsifying, centrifuging and freeze-drying to obtain the fast-energy milk fat microcapsules.

[0007] As a further improvement of the present invention, the following steps are included:

[0008] S1. Preparation of tea polyphenol / vitamin C fat-soluble substance: adding vitamin C and tea polyphenol to N,N-dimethylformamide, adding concentrated sulfuric acid and gallic acid, heating for reaction, filtering the product, washing, drying, and recrystallizing with anhydrous ethanol to obtain tea polyphenol / vitamin C fat-soluble substance;

[0009] S2. Processing of the core material: deep-sea fish oil, linseed oil and coconut oil are mixed evenly, compound lipase is added for enzymolysis, the enzyme is inactivated, tea polyphenols / vitamin C fat-soluble substances are added, and the mixture is stirred and mixed evenly to obtain the core material;

[0010] S3. Preparation of carboxylated chitosan: chitosan was dissolved in acid solution, pyruvic acid was added, the reaction was stirred, sodium borohydride was added, the reaction was continued, ethanol was added to terminate the reaction, filtered, washed, and dried to obtain carboxylated chitosan;

[0011] S4. Preparation of carboxylated chitosan - whey protein condensate; The carboxylated chitosan obtained in step S3 was activated with N-hydroxysuccinimide and 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide, and then reacted with whey protein to obtain a carboxylated chitosan - whey protein condensate;

[0012] S5. Preparation of fast-energy milk fat microcapsules: Sodium alginate, konjac glucomannan and carboxymethyl chitosan-whey protein condensate prepared in step S4 are mixed and added into water, and an emulsifier is added, and the mixture is stirred to obtain an aqueous phase. The core material prepared in step S1 is added dropwise into the obtained aqueous phase, emulsified, centrifuged, and freeze-dried to obtain fast-energy milk fat microcapsules.

[0013] As a further improvement of the present invention, the mass ratio of vitamin C, tea polyphenols, concentrated sulfuric acid and gallic acid in step S1 is 7-9:3-5:0.5-1:9-12, the temperature of the heating reaction is 110-120°C, and the time is 5-7h.

[0014] As a further improvement of the present invention, the mass ratio of deep-sea fish oil, linseed oil, coconut oil, compound lipase, and tea polyphenols / vitamin C fat-soluble substance in step S2 is 15-20:12-15:7-10:2-4:2-3, the compound lipase includes feed lipase and pancreatic lipase in a mass ratio of 5-7:7-10, the temperature of the enzymatic hydrolysis is 35-40°C, and the time is 2-4h.

[0015] As a further improvement of the present invention, in step S3, the mass ratio of chitosan, pyruvic acid and sodium borohydride is 10:4-6:2-3, the acid solution is 1-3wt% acetic acid or lactic acid solution, the stirring reaction temperature is 35-40°C, the time is 10-15h, the continued reaction time is 4-7h, and ethanol is added until the ethanol content of the system is 70-80wt%.

[0016] As a further improvement of the present invention, the mass ratio of carboxylated chitosan, N-hydroxysuccinimide, 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide and whey protein in step S4 is 10:3-5:5-7:3-5, the activation temperature is 0-4°C, the time is 20-40min, and the reaction time is 13-17h.

[0017] As a further improvement of the present invention, the mass ratio of sodium alginate, konjac glucomannan, carboxymethyl chitosan-whey protein condensate, emulsifier, water and core material in step S5 is 10-15:7-10:12-17:1-2:300-500:100-120, and the emulsifier is selected from at least one of Tween-20, Tween-40, Tween-60 and Tween-80.

[0018] As a further improvement of the present invention, the present invention specifically comprises the following steps:

[0019] S1. Preparation of tea polyphenol / vitamin C fat-soluble product: add 7-9 parts by weight of vitamin C and 3-5 parts by weight of tea polyphenol to 60-70 parts by weight of N,N-dimethylformamide, add 0.5-1 parts by weight of concentrated sulfuric acid and 9-12 parts by weight of gallic acid, heat to 110-120°C, stir and react for 5-7h, filter the product, wash, dry, and recrystallize with anhydrous ethanol to obtain tea polyphenol / vitamin C fat-soluble product;

[0020] S2. Treatment of the core material: 15-20 parts by weight of deep-sea fish oil, 12-15 parts by weight of linseed oil, and 7-10 parts by weight of coconut oil were mixed evenly, 2-4 parts by weight of composite lipase were added, and the enzyme was hydrolyzed at 35-40 ° C for 2-4h, the enzyme was inactivated, 2-3 parts by weight of tea polyphenols / vitamin C fat-soluble matter was added, and the mixture was stirred and mixed evenly to obtain a core material;

[0021] The composite lipase comprises feed lipase and pancreatic lipase in a mass ratio of 5-7:7-10;

[0022] S3. Preparation of carboxylated chitosan: 10 parts by weight of chitosan was dissolved in 200 parts by weight of 1-3wt% acetic acid or lactic acid solution, 4-6 parts by weight of pyruvic acid was added, the reaction was stirred at 35-40°C for 10-15h, 2-3 parts by weight of sodium borohydride was added, the reaction was continued for 4-7h, ethanol was added until the ethanol content of the system was 70-80wt%, the reaction was terminated, filtered, washed, and dried to obtain carboxylated chitosan;

[0023] S4. Preparation of carboxylated chitosan-whey protein condensate; add 10 parts by weight of carboxylated chitosan obtained in step S3 to 200 parts by weight of water, add 3-5 parts by weight of N-hydroxysuccinimide and 5-7 parts by weight of 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide, activate with stirring at 0-4°C for 20-40min, add 3-5 parts by weight of silk fibroin peptide, react with stirring at room temperature for 13-17h, add ethanol until the ethanol content of the system is 70-80wt%, terminate the reaction, filter, wash, and dry to obtain carboxylated chitosan-silk fibroin peptide condensate;

[0024] S5. Preparation of fast-energy milk fat microcapsules: mix 10-15 parts by weight of sodium alginate, 7-10 parts by weight of konjac glucomannan and 12-17 parts by weight of carboxymethyl chitosan-whey protein condensate obtained in step S4, add them into 300-500 parts by weight of water, add 1-2 parts by weight of emulsifier, stir and mix evenly to obtain an aqueous phase, dropwise add 100-120 parts by weight of the core material obtained in step S1 into the obtained aqueous phase, emulsify, centrifuge, and freeze-dry to obtain fast-energy milk fat microcapsules.

[0025] The present invention further protects a fast-energy milk fat microcapsule prepared by the above-mentioned preparation method.

[0026] The present invention further protects the use of the above-mentioned fast-energy milk fat microcapsules in preparing products that promote the growth of poultry and animals.

[0027] The present invention has the following beneficial effects:

[0028] The present invention prepares tea polyphenol / vitamin C fat-soluble substances, so that water-soluble tea polyphenol and vitamin C are modified into fat-soluble tea polyphenol and vitamin C, and their solubility in the oil phase is increased, thereby enhancing the antioxidant properties of tea polyphenol and vitamin C. At the same time, since vitamin C has a strong reducibility and is easily destroyed by oxidants and heat, light, trace heavy metals or fluorescent substances can promote its oxidation, so that the application of vitamin C is limited. The tea polyphenol / vitamin C fat-soluble substances prepared by the present invention also enhance the stability of vitamin C and can better exert the physiological function of vitamin C.

[0029] The deep-sea fish oil, linseed oil and coconut oil of the cream material of the present invention have good nutritional value, but because the structural oil is rich in unsaturated fatty acids, it is easy to oxidize and deteriorate, so it needs to be embedded, and the barrier property of the wall material is required to be good. In addition, adding tea polyphenols / vitamin C fat-soluble substances to the core material can well inhibit its oxidation and improve its storage stability. At the same time, the cream also has the problem of being difficult to absorb. After lipase enzymolysis, it is degraded into small molecular fatty acids that are easy to absorb, which greatly improves the absorption rate of the cream material and better promotes the growth of poultry and livestock.

[0030] The invention prepares carboxylated chitosan, which solves the disadvantage of chitosan being poorly soluble in water on the one hand, and on the other hand, the embedding shell formed by the prepared carboxylated chitosan has good acid resistance, can protect the active protein peptide of the inclusion from being destroyed by gastric acid, and has amphiphilicity, showing good emulsification characteristics and emulsification stability. Whey protein also contains a small amount of lactoperoxidase, growth factor, etc., has certain biological activity, is a high-quality full-price protein, and has low lactose, fat and cholesterol content, is very easy to digest and absorb, can promote health, improve immunity, and resist oxidation, inflammation, disease, etc. While whey protein has high nutritional value, its molecules have hydrophilic groups and hydrophobic groups, which make it have excellent surface activity and emulsification stability. Therefore, the prepared carboxylated chitosan-whey protein condensate is easy to form a film and is suitable as a wall material for microencapsulation to protect the stability of substances that are easily volatile and oxidizable. At the same time, since the prepared carboxylated chitosan-whey protein condensate has good emulsification, the prepared microcapsules are uniform in size, small in size, and easy to absorb and eat.

[0031] Wall materials such as sodium alginate and konjac glucomannan have no emulsifying properties and poor film-forming properties. When used alone, they have low microencapsulation efficiency and poor stability. However, using them in combination with carboxymethyl chitosan-whey protein condensate can effectively improve the embedding rate and meet the requirements of microcapsule preparation.

[0032] The fast-energy milk fat microcapsules prepared by the invention are uniform in size, small in size, easy to absorb and eat, have good fluidity, long shelf life, are extremely easy to digest and absorb, can promote physical health, promote the growth and development of poultry and livestock, improve immunity, resist oxidation, inflammation, disease, etc., and have broad application prospects. DETAILED DESCRIPTION

[0033] The technical solutions in the embodiments of the present invention are described clearly and completely below. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of them. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0034] Feed lipase, 100,000 U / g, was purchased from Xiasheng (Beijing) Biotechnology Development Co., Ltd. Pancreatic lipase, derived from porcine pancreas, 125,000 U / g, was purchased from Merck Life Sciences.

[0035] Chitosan, industrial grade, was purchased from Shandong Yatu Biotechnology Co., Ltd.; silk fibroin peptide, CAS: 96690-41-4, was purchased from Wuhan Huaxiang Kejie Biotechnology Co., Ltd.

[0036] Example 1

[0037] This embodiment provides a method for preparing fast energy milk fat microcapsules, which specifically comprises the following steps:

[0038] S1. Preparation of tea polyphenol / vitamin C fat-soluble product: 7 parts by weight of vitamin C and 3 parts by weight of tea polyphenol are added to 60 parts by weight of N,N-dimethylformamide, 0.5 parts by weight of concentrated sulfuric acid and 9 parts by weight of gallic acid are added, heated to 110°C, stirred for reaction for 5 hours, the product is filtered, washed, dried, and recrystallized with anhydrous ethanol to obtain tea polyphenol / vitamin C fat-soluble product;

[0039] S2. Treatment of the core material: 15 parts by weight of deep-sea fish oil, 12 parts by weight of linseed oil, and 7 parts by weight of coconut oil were mixed evenly, 2 parts by weight of composite lipase were added, and the enzyme was hydrolyzed at 35°C for 2h, the enzyme was inactivated, 2 parts by weight of tea polyphenols / vitamin C fat-soluble was added, and the mixture was stirred for 20min to obtain a core material;

[0040] The composite lipase comprises feed lipase and pancreatic lipase in a mass ratio of 5:7;

[0041] S3. Preparation of carboxylated chitosan: 10 parts by weight of chitosan was dissolved in 200 parts by weight of 1 wt% acetic acid solution, 4 parts by weight of pyruvic acid was added, the reaction was stirred at 35 ° C for 10 h, 2 parts by weight of sodium borohydride was added, the reaction was continued for 4 h, ethanol was added until the ethanol content of the system was 70 wt%, the reaction was terminated, filtered, washed, and dried to obtain carboxylated chitosan;

[0042] S4. Preparation of carboxylated chitosan-whey protein condensate; add 10 parts by weight of the carboxylated chitosan obtained in step S3 to 200 parts by weight of water, add 3 parts by weight of N-hydroxysuccinimide and 5 parts by weight of 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide, activate with stirring at 0°C for 20 minutes, add 3 parts by weight of silk fibroin peptide, react with stirring at room temperature for 13 hours, add ethanol until the ethanol content of the system is 70wt%, terminate the reaction, filter, wash, and dry to obtain a carboxylated chitosan-silk fibroin peptide condensate;

[0043] S5. Preparation of fast-energy milk fat microcapsules: mix 10 parts by weight of sodium alginate, 7 parts by weight of konjac glucomannan and 12 parts by weight of carboxymethyl chitosan-whey protein condensate obtained in step S4, add into 300 parts by weight of water, add 1 part by weight of emulsifier Tween-20, stir and mix for 30 minutes to obtain an aqueous phase, dropwise add 100 parts by weight of the core material obtained in step S1 into the obtained aqueous phase, emulsify at 10,000 r / min for 15 minutes, centrifuge, and freeze-dry to obtain fast-energy milk fat microcapsules.

[0044] Example 2

[0045] This embodiment provides a method for preparing fast energy milk fat microcapsules, which specifically comprises the following steps:

[0046] S1. Preparation of tea polyphenol / vitamin C fat-soluble substance: 9 parts by weight of vitamin C and 5 parts by weight of tea polyphenol are added to 70 parts by weight of N,N-dimethylformamide, 1 part by weight of concentrated sulfuric acid and 12 parts by weight of gallic acid are added, heated to 120°C, stirred for reaction for 7 hours, the product is filtered, washed, dried, and recrystallized with anhydrous ethanol to obtain tea polyphenol / vitamin C fat-soluble substance;

[0047] S2. Treatment of the core material: 20 parts by weight of deep-sea fish oil, 15 parts by weight of linseed oil, and 10 parts by weight of coconut oil were mixed evenly, 4 parts by weight of composite lipase were added, enzymatic hydrolysis was carried out at 40°C for 4h, the enzyme was inactivated, 3 parts by weight of tea polyphenols / vitamin C fat-soluble substance were added, and the mixture was stirred for 20min to obtain a core material;

[0048] The composite lipase comprises feed lipase and pancreatic lipase in a mass ratio of 7:10;

[0049] S3. Preparation of carboxylated chitosan: 10 parts by weight of chitosan was dissolved in 200 parts by weight of 3 wt% lactic acid solution, 6 parts by weight of pyruvic acid was added, the reaction was stirred at 40 ° C for 15 h, 3 parts by weight of sodium borohydride was added, the reaction was continued for 7 h, ethanol was added to the system ethanol content of 80 wt%, the reaction was terminated, filtered, washed, and dried to obtain carboxylated chitosan;

[0050] S4. Preparation of carboxylated chitosan-whey protein condensate; add 10 parts by weight of carboxylated chitosan obtained in step S3 to 200 parts by weight of water, add 5 parts by weight of N-hydroxysuccinimide and 7 parts by weight of 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide, activate with stirring at 4°C for 40 minutes, add 5 parts by weight of silk fibroin peptide, react with stirring at room temperature for 17 hours, add ethanol until the ethanol content of the system is 80wt%, terminate the reaction, filter, wash, and dry to obtain carboxylated chitosan-silk fibroin peptide condensate;

[0051] S5. Preparation of fast-energy milk fat microcapsules: Mix 15 parts by weight of sodium alginate, 10 parts by weight of konjac glucomannan and 17 parts by weight of carboxymethyl chitosan-whey protein condensate obtained in step S4, add into 500 parts by weight of water, add 2 parts by weight of emulsifier Tween-40, stir and mix for 30 minutes to obtain an aqueous phase, dropwise add 120 parts by weight of the core material obtained in step S1 into the obtained aqueous phase, emulsify at 10,000 r / min for 15 minutes, centrifuge, and freeze-dry to obtain fast-energy milk fat microcapsules.

[0052] Example 3

[0053] This embodiment provides a method for preparing fast energy milk fat microcapsules, which specifically comprises the following steps:

[0054] S1. Preparation of tea polyphenol / vitamin C fat-soluble substance: 8 parts by weight of vitamin C and 4 parts by weight of tea polyphenol are added to 65 parts by weight of N,N-dimethylformamide, 0.7 parts by weight of concentrated sulfuric acid and 10 parts by weight of gallic acid are added, and the mixture is heated to 115°C and stirred for reaction for 6 hours. The product is filtered, washed, dried, and recrystallized with anhydrous ethanol to obtain tea polyphenol / vitamin C fat-soluble substance;

[0055] S2. Treatment of the core material: 17 parts by weight of deep-sea fish oil, 13.5 parts by weight of linseed oil, and 8.5 parts by weight of coconut oil were mixed evenly, 3 parts by weight of composite lipase were added, and the enzyme was hydrolyzed at 37°C for 3h, the enzyme was inactivated, 2.5 parts by weight of tea polyphenols / vitamin C fat-soluble was added, and the mixture was stirred for 20min to obtain a core material;

[0056] The composite lipase comprises feed lipase and pancreatic lipase in a mass ratio of 6:9;

[0057] S3. Preparation of carboxylated chitosan: 10 parts by weight of chitosan was dissolved in 200 parts by weight of 2wt% acetic acid solution, 5 parts by weight of pyruvic acid was added, the reaction was stirred at 37°C for 12h, 2.5 parts by weight of sodium borohydride was added, the reaction was continued for 6h, ethanol was added until the ethanol content of the system was 75wt%, the reaction was terminated, filtered, washed, and dried to obtain carboxylated chitosan;

[0058] S4. Preparation of carboxylated chitosan-whey protein condensate; add 10 parts by weight of carboxylated chitosan obtained in step S3 to 200 parts by weight of water, add 4 parts by weight of N-hydroxysuccinimide and 6 parts by weight of 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide, activate with stirring at 2°C for 30 minutes, add 4 parts by weight of silk fibroin peptide, react with stirring at room temperature for 15 hours, add ethanol until the ethanol content of the system is 75wt%, terminate the reaction, filter, wash, and dry to obtain carboxylated chitosan-silk fibroin peptide condensate;

[0059] S5. Preparation of fast-energy milk fat microcapsules: Mix 12 parts by weight of sodium alginate, 8.5 parts by weight of konjac glucomannan and 15 parts by weight of carboxymethyl chitosan-whey protein condensate obtained in step S4, add into 400 parts by weight of water, add 1.5 parts by weight of emulsifier Tween-80, stir and mix for 30 minutes to obtain an aqueous phase, dropwise add 110 parts by weight of the core material obtained in step S1 into the obtained aqueous phase, emulsify at 10,000 r / min for 15 minutes, centrifuge, and freeze-dry to obtain fast-energy milk fat microcapsules.

[0060] Example 4

[0061] Compared with Example 3, the difference is that the composite lipase is a single feed lipase.

[0062] Example 5

[0063] Compared with Example 3, the difference is that the composite lipase is a single pancreatic lipase.

[0064] Comparative Example 1

[0065] Compared with Example 3, the difference is that vitamin C is not added in step S1.

[0066] The details are as follows:

[0067] S1. Preparation of fat-soluble tea polyphenols: Add 12 parts by weight of tea polyphenols to 65 parts by weight of N,N-dimethylformamide, add 0.7 parts by weight of concentrated sulfuric acid and 10 parts by weight of gallic acid, heat to 115°C, stir and react for 6 hours, filter the product, wash, dry, and recrystallize with anhydrous ethanol to obtain fat-soluble tea polyphenols.

[0068] Comparative Example 2

[0069] Compared with Example 3, the difference is that tea polyphenols are not added in step S1.

[0070] The details are as follows:

[0071] S1. Preparation of fat-soluble vitamin C: Add 12 parts by weight of vitamin C to 65 parts by weight of N,N-dimethylformamide, add 0.7 parts by weight of concentrated sulfuric acid and 10 parts by weight of gallic acid, heat to 115°C, stir to react for 6 hours, filter the product, wash, dry, and recrystallize with anhydrous ethanol to obtain fat-soluble vitamin C.

[0072] Comparative Example 3

[0073] Compared with Example 3, the difference is that no composite lipase is added in step S2.

[0074] The details are as follows:

[0075] S2. Processing of the core material: 17 parts by weight of deep-sea fish oil, 13.5 parts by weight of linseed oil, and 8.5 parts by weight of coconut oil were evenly mixed, and 2.5 parts by weight of tea polyphenols / vitamin C fat-soluble substance were added, and stirred for 20 minutes to obtain the core material.

[0076] Comparative Example 4

[0077] Compared with Example 3, the difference is that tea polyphenols / vitamin C fat-soluble substances are not added in step S2.

[0078] The details are as follows:

[0079] S2. Treatment of the core material: 17 parts by weight of deep-sea fish oil, 13.5 parts by weight of linseed oil, and 8.5 parts by weight of coconut oil were mixed uniformly, 3 parts by weight of composite lipase were added, and the enzyme was hydrolyzed at 37°C for 3h, and the enzyme was inactivated to obtain a core material;

[0080] The composite lipase comprises feed lipase and pancreatic lipase in a mass ratio of 6:9.

[0081] Comparative Example 5

[0082] Compared with Example 3, the difference is that step S3 is not performed.

[0083] The details are as follows:

[0084] S1. Preparation of tea polyphenol / vitamin C fat-soluble substance: 8 parts by weight of vitamin C and 4 parts by weight of tea polyphenol are added to 65 parts by weight of N,N-dimethylformamide, 0.7 parts by weight of concentrated sulfuric acid and 10 parts by weight of gallic acid are added, and the mixture is heated to 115°C and stirred for reaction for 6 hours. The product is filtered, washed, dried, and recrystallized with anhydrous ethanol to obtain tea polyphenol / vitamin C fat-soluble substance;

[0085] S2. Treatment of the core material: 17 parts by weight of deep-sea fish oil, 13.5 parts by weight of linseed oil, and 8.5 parts by weight of coconut oil were mixed evenly, 3 parts by weight of composite lipase were added, and the enzyme was hydrolyzed at 37°C for 3h, the enzyme was inactivated, 2.5 parts by weight of tea polyphenols / vitamin C fat-soluble was added, and the mixture was stirred for 20min to obtain a core material;

[0086] The composite lipase comprises feed lipase and pancreatic lipase in a mass ratio of 6:9;

[0087] S3. Preparation of chitosan-whey protein condensate; 10 parts by weight of chitosan was added to 200 parts by weight of water, 4 parts by weight of N-hydroxysuccinimide and 6 parts by weight of 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide were added, and the mixture was stirred at 2°C for 30 minutes for activation, 4 parts by weight of silk fibroin peptide were added, and the mixture was stirred at room temperature for 15 hours for reaction, ethanol was added until the ethanol content of the system was 75wt%, the reaction was terminated, filtered, washed, and dried to obtain a carboxylated chitosan-silk fibroin peptide condensate;

[0088] S4. Preparation of fast-energy milk fat microcapsules: Mix 12 parts by weight of sodium alginate, 8.5 parts by weight of konjac glucomannan and 15 parts by weight of chitosan-whey protein condensate obtained in step S3, add into 400 parts by weight of water, add 1.5 parts by weight of emulsifier Tween-80, stir and mix for 30 minutes to obtain an aqueous phase, dropwise add 110 parts by weight of the core material obtained in step S1 into the obtained aqueous phase, emulsify at 10,000 r / min for 15 minutes, centrifuge, and freeze-dry to obtain fast-energy milk fat microcapsules.

[0089] Comparative Example 6

[0090] Compared with Example 3, the difference is that step S4 is not performed.

[0091] The details are as follows:

[0092] S1. Preparation of tea polyphenol / vitamin C fat-soluble substance: 8 parts by weight of vitamin C and 4 parts by weight of tea polyphenol are added to 65 parts by weight of N,N-dimethylformamide, 0.7 parts by weight of concentrated sulfuric acid and 10 parts by weight of gallic acid are added, and the mixture is heated to 115°C and stirred for reaction for 6 hours. The product is filtered, washed, dried, and recrystallized with anhydrous ethanol to obtain tea polyphenol / vitamin C fat-soluble substance;

[0093] S2. Treatment of the core material: 17 parts by weight of deep-sea fish oil, 13.5 parts by weight of linseed oil, and 8.5 parts by weight of coconut oil were mixed evenly, 3 parts by weight of composite lipase were added, and the enzyme was hydrolyzed at 37°C for 3h, the enzyme was inactivated, 2.5 parts by weight of tea polyphenols / vitamin C fat-soluble was added, and the mixture was stirred for 20min to obtain a core material;

[0094] The composite lipase comprises feed lipase and pancreatic lipase in a mass ratio of 6:9;

[0095] S3. Preparation of carboxylated chitosan: 10 parts by weight of chitosan was dissolved in 200 parts by weight of 2wt% acetic acid solution, 5 parts by weight of pyruvic acid was added, the reaction was stirred at 37°C for 12h, 2.5 parts by weight of sodium borohydride was added, the reaction was continued for 6h, ethanol was added until the ethanol content of the system was 75wt%, the reaction was terminated, filtered, washed, and dried to obtain carboxylated chitosan;

[0096] S4. Preparation of fast-energy cream microcapsules: Mix 12 parts by weight of sodium alginate, 8.5 parts by weight of konjac glucomannan and 15 parts by weight of carboxymethyl chitosan obtained in step S3 and add them to 400 parts by weight of water, add 1.5 parts by weight of emulsifier Tween-80, stir and mix for 30 minutes to obtain an aqueous phase, dropwise add 110 parts by weight of the core material obtained in step S1 into the obtained aqueous phase, emulsify at 10,000 r / min for 15 minutes, centrifuge, and freeze-dry to obtain fast-energy cream microcapsules.

[0097] Comparative Example 7

[0098] Compared with Example 3, the difference is that no carboxymethyl chitosan-whey protein condensate is added in step S5.

[0099] The details are as follows:

[0100] S5. Preparation of fast-energy cream microcapsules: Mix 27 parts by weight of sodium alginate and 8.5 parts by weight of konjac glucomannan and add them to 400 parts by weight of water, add 1.5 parts by weight of emulsifier Tween-80, stir and mix for 30 minutes to obtain an aqueous phase, dropwise add 110 parts by weight of the core material obtained in step S1 into the obtained aqueous phase, emulsify at 10,000 r / min for 15 minutes, centrifuge, and freeze-dry to obtain fast-energy cream microcapsules.

[0101] Test Example 1 Determination of embedding rate

[0102] Embedding rate (%) = (1-microcapsule surface oil content / microcapsule total oil content) × 100%

[0103] Determination of microcapsule surface oil: Using petroleum ether as solvent, accurately weigh (m1) the fast-energy milk fat microcapsules prepared in Examples 1-5 and Comparative Examples 1-7 into a dry bottle (m2), add 50 mL of petroleum ether, and extract for 5 minutes to avoid damage to the microcapsules. Filter the sample with filter paper (m3) and wash twice with petroleum ether. Dry the bottle and filter paper to constant weight (m4).

[0104] Surface oil = (m1+m2+m3-m4) / m1

[0105] Determination of total oil in microcapsules: Mix anhydrous ethanol, anhydrous ether and petroleum ether in a volume ratio of 2:1:1, use the mixed solution as the solvent, accurately weigh (m1) microcapsule powder in dry medium, add hot water to dissolve, add the mixed solvent to fully extract for 10 minutes, transfer the extract to a weighed rotary evaporator (m2), repeat the extraction 3 times, combine the extracts, spin dry the solvent, and dry to constant weight (m3).

[0106] Total oil content = (m3-m2) / m1

[0107] The results are shown in Table 1.

[0108] Table 1

[0109] Group Embedding rate (%) Example 1 95.6 Example 2 96.1 Example 3 96.7 Example 4 94.2 Example 5 93.9 Comparative Example 1 95.0 Comparative Example 2 94.8 Comparative Example 3 92.2 Comparative Example 4 93.7 Comparative Example 5 88.6 Comparative Example 6 84.5 Comparative Example 7 80.1

[0110] It can be seen from the above table that the fast energy milk fat microcapsules prepared in Examples 1-3 of the present invention have a higher embedding rate.

[0111] Test Example 2 Determination of Storage Stability

[0112] The milk fat microcapsules were placed in a sealed container and then stored in a constant temperature incubator at 20 and 40°C, respectively. The surface oil and total oil of the microcapsules were measured every 14 days (see Test Example 1 for the test method). The test lasted for 28 days, and the changes in the retention rate were analyzed. The results are shown in Table 2.

[0113] Table 2 Retention rate change (%)

[0114]

[0115] It can be seen from the above table that the fast energy milk fat microcapsules prepared in Examples 1-3 of the present invention have good storage stability.

[0116] Test Example 3

[0117] 270 healthy fattening pigs with an average initial weight of (68.44±0.94) kg were selected and randomly divided into 13 groups, each with 10 pigs (5 males and 5 females). The pre-test period was 5 days and the main test period was 30 days. The control group was fed a basic diet, and the experimental group was added with 200 mg / kg of the fast-energy milk fat microcapsules prepared in Examples 1-5 or Comparative Examples 1-7 to the basic diet. The pigs were raised in separate pens, immunized with normal procedures, raised according to routine management, and the pig houses were routinely disinfected. The experimental pigs were free to eat and drink water. The formula of the basic diet is as follows: 63.5wt% corn, 20wt% soybean meal, 8wt% wheat bran, 4.5wt% peanut cake, 1.4wt% calcium carbonate, 1.3wt% calcium bicarbonate, 0.3wt% salt, 1wt% premix, wherein each kilogram of premix contains: vitamin A 6200IU, vitamin D 3700IU, vitamin E 88IU, vitamin K (menadione sodium bisulfite complex) 4.4mg, vitamin B 28.8mg, pantothenic acid 24.2mg, niacin (nicotinic acid) 33mg, choline 330mg; copper 15mg (CuSO4·5H2O), zinc 105mg (ZnSO4·7H2O), iron 135mg (FeSO4·H2O), manganese 40mg (MnSO4·5H2O), selenium 0.15mg (Na2SeO3·5H2O), iodine 0.3mg (KI).

[0118] 1. Growth performance

[0119] The body weight of each replicate was measured at the beginning and end of the experiment, and the feed consumption of each replicate was recorded every day. The average daily gain (ADG), average daily feed intake (ADFI) and feed-to-weight ratio (F / G) were calculated. The results are shown in Table 1.

[0120] Table 1

[0121]

[0122] It can be seen from the above table that the cysteamine coated products prepared in Examples 1-3 of the present invention can significantly promote the growth of finishing pigs and improve the feed consumption to weight gain ratio.

[0123] 2. Serum immune indicators Serum immune indicators IgA, IgG, IgM

[0124] After the experiment, one boar and one sow with the closest average weight were selected from each replicate and fasted for 12 hours. 5 mL of anterior vena cava blood was collected and centrifuged to take the upper serum. The serum samples of each group of boars and sows were mixed evenly, and the serum immune indexes IgA, IgG, and IgM were determined using the corresponding kits. The results are shown in Table 2.

[0125] Table 2

[0126] Group IgA content (g / L) IgG content (g / L) IgM content (g / L) Control group 0.10 2.29 0.14 Example 1 0.11 3.12 0.24 Example 2 0.12 3.13 0.25 Example 3 0.11 3.15 0.27 Example 4 0.11 3.10 0.22 Example 5 0.10 3.08 0.21 Comparative Example 1 0.11 3.01 0.20 Comparative Example 2 0.12 2.98 0.21 Comparative Example 3 0.12 3.02 0.19 Comparative Example 4 0.13 2.94 0.17 Comparative Example 5 0.10 2.90 0.20 Comparative Example 6 0.11 2.88 0.18 Comparative Example 7 0.10 2.83 0.17

[0127] It can be seen from the above table that the cysteamine coated products prepared in Examples 1-3 of the present invention can significantly increase the content of IgG and IgM, but have no significant promoting effect on IgA.

[0128] The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention. Any modifications, equivalent substitutions, improvements, etc. made within the spirit and principle of the present invention should be included in the protection scope of the present invention.

Claims

1. A method for preparing fast energy milk fat microcapsules, characterized in that: Deep-sea fish oil, linseed oil and coconut oil are enzymatically hydrolyzed and then tea polyphenols / vitamin C fat-soluble substances are added to obtain a core material, which is then added to an aqueous solution containing sodium alginate, konjac glucomannan and the carboxymethyl chitosan-whey protein condensate obtained in step S4, emulsified, centrifuged and freeze-dried to obtain fast-energy milk fat microcapsules.

2. The preparation method according to claim 1, characterized in that: The following steps are involved: S1. Preparation of tea polyphenol / vitamin C fat-soluble substance: adding vitamin C and tea polyphenol to N,N-dimethylformamide, adding concentrated sulfuric acid and gallic acid, heating for reaction, filtering the product, washing, drying, and recrystallizing with anhydrous ethanol to obtain tea polyphenol / vitamin C fat-soluble substance; S2. Processing of the core material: deep-sea fish oil, linseed oil and coconut oil are mixed evenly, compound lipase is added for enzymolysis, the enzyme is inactivated, tea polyphenols / vitamin C fat-soluble substances are added, and the mixture is stirred and mixed evenly to obtain the core material; S3. Preparation of carboxylated chitosan: chitosan was dissolved in acid solution, pyruvic acid was added, the reaction was stirred, sodium borohydride was added, the reaction was continued, ethanol was added to terminate the reaction, filtered, washed, and dried to obtain carboxylated chitosan; S4. Preparation of carboxylated chitosan - whey protein condensate; The carboxylated chitosan obtained in step S3 was activated with N-hydroxysuccinimide and 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide, and then reacted with whey protein to obtain a carboxylated chitosan - whey protein condensate; S5. Preparation of fast-energy milk fat microcapsules: Sodium alginate, konjac glucomannan and carboxymethyl chitosan-whey protein condensate prepared in step S4 are mixed and added into water, and an emulsifier is added, and the mixture is stirred to obtain an aqueous phase. The core material prepared in step S1 is added dropwise into the obtained aqueous phase, emulsified, centrifuged, and freeze-dried to obtain fast-energy milk fat microcapsules.

3. The preparation method according to claim 2, characterized in that: In step S1, the mass ratio of vitamin C, tea polyphenols, concentrated sulfuric acid and gallic acid is 7-9:3-5:0.5-1:9-12, the temperature of the heating reaction is 110-120°C, and the time is 5-7h.

4. The preparation method according to claim 2, characterized in that: The mass ratio of deep-sea fish oil, linseed oil, coconut oil, compound lipase, and tea polyphenols / vitamin C fat-soluble substance in step S2 is 15-20:12-15:7-10:2-4:2-3, the compound lipase includes feed lipase and pancreatic lipase in a mass ratio of 5-7:7-10, the temperature of the enzymolysis is 35-40°C, and the time is 2-4h.

5. The preparation method according to claim 2, characterized in that: In step S3, the mass ratio of chitosan, pyruvic acid and sodium borohydride is 10:4-6:2-3, the acid solution is 1-3wt% acetic acid or lactic acid solution, the stirring reaction temperature is 35-40°C, the time is 10-15h, the continued reaction time is 4-7h, and ethanol is added until the ethanol content of the system is 70-80wt%.

6. The preparation method according to claim 2, characterized in that: In step S4, the mass ratio of carboxylated chitosan, N-hydroxysuccinimide, 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide and whey protein is 10:3-5:5-7:3-5, the activation temperature is 0-4°C, the time is 20-40min, and the reaction time is 13-17h.

7. The preparation method according to claim 2, characterized in that: In step S5, the mass ratio of sodium alginate, konjac glucomannan, carboxymethyl chitosan-whey protein condensate, emulsifier, water and core material is 10-15:7-10:12-17:1-2:300-500:100-120, and the emulsifier is selected from at least one of Tween-20, Tween-40, Tween-60 and Tween-80.

8. The preparation method according to claim 2, characterized in that: The specific steps include: S1. Preparation of tea polyphenol / vitamin C fat-soluble product: add 7-9 parts by weight of vitamin C and 3-5 parts by weight of tea polyphenol to 60-70 parts by weight of N,N-dimethylformamide, add 0.5-1 parts by weight of concentrated sulfuric acid and 9-12 parts by weight of gallic acid, heat to 110-120°C, stir and react for 5-7h, filter the product, wash, dry, and recrystallize with anhydrous ethanol to obtain tea polyphenol / vitamin C fat-soluble product; S2. Treatment of the core material: 15-20 parts by weight of deep-sea fish oil, 12-15 parts by weight of linseed oil, and 7-10 parts by weight of coconut oil were mixed evenly, 2-4 parts by weight of composite lipase were added, and the enzyme was hydrolyzed at 35-40 ° C for 2-4h, the enzyme was inactivated, 2-3 parts by weight of tea polyphenols / vitamin C fat-soluble matter was added, and the mixture was stirred and mixed evenly to obtain a core material; The composite lipase comprises feed lipase and pancreatic lipase in a mass ratio of 5-7:7-10; S3. Preparation of carboxylated chitosan: 10 parts by weight of chitosan was dissolved in 200 parts by weight of 1-3wt% acetic acid or lactic acid solution, 4-6 parts by weight of pyruvic acid was added, the reaction was stirred at 35-40°C for 10-15h, 2-3 parts by weight of sodium borohydride was added, the reaction was continued for 4-7h, ethanol was added until the ethanol content of the system was 70-80wt%, the reaction was terminated, filtered, washed, and dried to obtain carboxylated chitosan; S4. Preparation of carboxylated chitosan-whey protein condensate; add 10 parts by weight of carboxylated chitosan obtained in step S3 to 200 parts by weight of water, add 3-5 parts by weight of N-hydroxysuccinimide and 5-7 parts by weight of 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide, activate with stirring at 0-4°C for 20-40min, add 3-5 parts by weight of silk fibroin peptide, react with stirring at room temperature for 13-17h, add ethanol until the ethanol content of the system is 70-80wt%, terminate the reaction, filter, wash, and dry to obtain carboxylated chitosan-silk fibroin peptide condensate; S5. Preparation of fast-energy milk fat microcapsules: mix 10-15 parts by weight of sodium alginate, 7-10 parts by weight of konjac glucomannan and 12-17 parts by weight of carboxymethyl chitosan-whey protein condensate obtained in step S4, add them into 300-500 parts by weight of water, add 1-2 parts by weight of emulsifier, stir and mix evenly to obtain an aqueous phase, dropwise add 100-120 parts by weight of the core material obtained in step S1 into the obtained aqueous phase, emulsify, centrifuge, and freeze-dry to obtain fast-energy milk fat microcapsules.

9. A fast-energy milk fat microcapsule prepared by the preparation method according to any one of claims 1 to 8.

10. Use of the fast-energy milk fat microcapsules as claimed in claim 9 in preparing products that promote the growth of poultry and animals.

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