Production method and application of feed emulsifier with high content of lysolecithin
By using high-content lyselcithin in feed emulsifiers, synergistically interacts with other fatty acid esters, the problems of easy deactivation and poor emulsification stability of existing emulsifiers in high-temperature processing are solved, efficient fat digestion and utilization is achieved, diarrhea is prevented, and the digestion and absorption efficiency of feed is improved.
Patent Information
- Application Number
- CN202510378724.8
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-03-28
- Publication Date
- 2025-05-16
AI Technical Summary
Existing feed emulsifiers are prone to inactivate during high-temperature processing, have poor emulsification stability, and long-term use will inhibit the secretion of digestive enzymes and affect animal health.
High-content lysecithin is used to synergize with sucrose fatty acid esters, taurine, glyceryl monostearate, polyglycerol fatty acid esters, etc., and through specific mixing and treatment methods, the emulsification performance and stability of the emulsifier are improved.
It significantly improves the digestive utilization rate of fat, prevents diarrhea from animals, and maintains emulsification activity under high temperature conditions, improving the digestive and absorption efficiency of feed.
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Abstract
Description
Technical Field
[0001] The invention belongs to the technical field of animal feed emulsifiers, and in particular relates to a production method and application of a feed emulsifier with a high content of lysolecithin. Background Art
[0002] With the development of intensive animal husbandry, the feed industry usually adopts a high-proportion oil addition strategy to improve energy density and breeding efficiency. However, due to the immature digestive system of young livestock and poultry, bile salts and lipase secretion are insufficient, making it difficult to effectively emulsify and absorb fat, resulting in oil waste and even diarrhea and other production losses. As a water-insoluble substance, fat needs to be emulsified to form chylomicrons before it can be digested and absorbed. This characteristic has given rise to the market demand for feed emulsifiers. The current mainstream emulsifiers include phospholipids, glycerides and bile salts. These emulsifiers can not only help improve the physical properties of feed, but also have certain physiological activities, such as enhancing intestinal health and regulating immune function. However, each of them also has some disadvantages. Among them, phospholipid emulsifiers are easily inactivated during high-temperature processing, and need to be converted into lysolecithin to work, and their conversion efficiency is also poor. The oil-water complex formed by glyceride emulsifiers has a larger particle size, which will affect its emulsification efficiency and fat absorption effect. Long-term use of bile salt emulsifiers will inhibit the secretion of endogenous digestive enzymes through the enterohepatic circulation, thereby exacerbating the degradation of digestive function and having an adverse effect on animal health. In addition, traditional emulsifiers generally have problems such as single ingredients, low emulsification stability, and inability to continuously participate in the fat digestion process, resulting in limited improvement in fat utilization.
[0003] Compared with ordinary phospholipids, lysophosphatidylcholine has a unique molecular structure advantage. Its conical molecular structure enhances hydrophilicity by reducing hydrophobic groups, and the oil-water complex formed has a smaller particle size. At the same time, it has better thermal stability and can withstand higher processing temperatures. It can also directly participate in the formation of microbubble structures to promote fatty acid absorption, and the emulsification efficiency is significantly improved. Chinese patent CN104212849A discloses a method for preparing lysophospholipids, including the following steps: taking powdered phospholipids, dissolving them with Tris-HCl buffer to obtain a phospholipid solution, then adding calcium chloride, heating and adding phospholipase A2 to react, and performing chromatography after the reaction is completed to obtain; the lysophospholipid process of the patent is simple and has a high recovery rate, which is suitable for industrial production. Chinese patent CN114698734A discloses a kind of lysolecithin for feeding and its preparation method, feed emulsifier and its preparation method, the preparation method of the lysolecithin for feeding is: after preheating soybean lecithin, add water and phospholipase in sequence, heat and keep warm for enzymolysis, and heat up and kill enzyme after the enzymolysis is completed, and obtain; the lysolecithin of this patent can promote the digestion and absorption of fat by poultry and livestock as a feed additive, and its enzymolysis yield is also improved, which reduces the production cost to a certain extent. Although the above patent discloses different methods for preparing lysolecithin by enzymolysis, there are still problems such as low content of lysophosphatidylcholine and insufficient hydrophilicity in the product. Therefore, it is urgent to develop a method for producing a high-content lysolecithin feed emulsifier with excellent comprehensive performance. Summary of the invention
[0004] In view of the shortcomings of the prior art, the present invention provides a method for producing a feed emulsifier with a high content of lysolecithin, by adopting the synergistic effect of specific lysolecithin and sucrose fatty acid ester, taurine, glyceryl monostearate, polyglycerol fatty acid ester, etc., to further improve the emulsification performance and emulsification stability of the emulsifier.
[0005] The technical solution adopted by the present invention is:
[0006] The present invention provides a method for producing a feed emulsifier containing high content of lysolecithin, comprising the following steps:
[0007] S1. Mix 50-70 parts by weight of lysolecithin, 10-20 parts by weight of sucrose fatty acid ester, 1-3 parts by weight of taurine, 3-6 parts by weight of silicon dioxide and 150-250 parts by weight of sodium alginate aqueous solution, heat and stir to obtain a water phase; mix 7-12 parts by weight of glyceryl monostearate and 10-15 parts by weight of polyglycerol fatty acid ester, heat and stir to obtain an oil phase;
[0008] S2. 15-25 parts by weight of the oil phase and 150-200 parts by weight of the water phase are combined, and the mixture is subjected to high-speed shearing and high-pressure homogenization in sequence. Then, 2-5 parts by weight of the coated antioxidant is added, stirred, spray-dried, and sieved to obtain the feed emulsifier containing a high content of lysolecithin.
[0009] Preferably, the coated antioxidant is prepared by the following method:
[0010] 0.5-1.5 parts by weight of ascorbyl glucoside and 40-60 parts by weight of hydroxypropyl-β-cyclodextrin aqueous solution are mixed, heated and stirred, concentrated under reduced pressure, and freeze-dried to obtain a coated antioxidant.
[0011] The feed emulsifier produced by the present invention adopts the above method, and its emulsifying performance is significantly improved by optimizing different raw materials. Among them, lysolecithin, as one of the main active ingredients, can be quickly adsorbed on the oil-water interface and reduce the interfacial tension, promoting the formation of stable small-sized emulsion droplets. Sucrose fatty acid esters work together with glyceryl monostearate and polyglycerol fatty acid esters to further enhance the stability of the emulsification system. In addition, sodium alginate helps to form a more stable emulsion structure, and can protect the emulsifier from the influence of digestive enzymes in the gastrointestinal tract to maintain emulsification activity. Silicon dioxide, as a glidant, can improve the fluidity of the emulsion and reduce coagulation. Taurine, as a nutritional factor, participates in enhancing the digestion and absorption of feed during the digestion process and improves feed utilization efficiency.
[0012] The present invention also uses hydroxypropyl-β-cyclodextrin to coat ascorbyl glucoside to achieve sustained release of antioxidants, and then cooperates with freeze-drying process to form a porous structure, dissipating energy through endothermic phase change during high-temperature granulation (80-120°C), thereby extending the phosphatidyl oxidation induction time. At the same time, sodium alginate and silicon dioxide form a three-dimensional network skeleton, and the molecular conformation of the emulsifier is fixed by hydrogen bonds and van der Waals forces during the spray drying process, thereby improving high-temperature stability.
[0013] Preferably, a method for producing a feed emulsifier containing a high content of lysolecithin comprises the following steps:
[0014] S1. Mix 50-70 parts by weight of lysolecithin, 10-20 parts by weight of sucrose fatty acid ester, 1-3 parts by weight of taurine, 3-6 parts by weight of silicon dioxide and 150-250 parts by weight of sodium alginate aqueous solution, stir at 45-55° C. and 200-400 r / min for 20-30 min to obtain an aqueous phase; mix 7-12 parts by weight of glyceryl monostearate and 10-15 parts by weight of polyglycerol fatty acid ester, stir at 58-66° C. and 100-300 r / min for 10-20 min to obtain an oil phase; mix 0.5-1.5 parts by weight of ascorbyl glucoside and 40-60 parts by weight of hydroxypropyl-β-cyclodextrin aqueous solution, stir at 50-60° C. and 100-300 r / min for 10-15 h, concentrate under reduced pressure to 15-25% of the original weight, and freeze-dry to obtain a coated antioxidant;
[0015] S2. 15-25 parts by weight of the oil phase and 150-200 parts by weight of the water phase are combined, and the mixture is subjected to high-speed shearing and high-pressure homogenization in sequence, and then 2-5 parts by weight of a coated antioxidant is added, and the mixture is stirred at 23-27° C. and 200-400 r / min for 3-7 min, spray-dried, and sieved through a 60-100 mesh screen to obtain the feed emulsifier containing a high content of lysolecithin.
[0016] Preferably, the concentration of the sodium alginate aqueous solution is 1-3wt%.
[0017] Preferably, the concentration of the hydroxypropyl-β-cyclodextrin aqueous solution is 7-12 wt %.
[0018] Preferably, the high-speed shearing conditions are: high-speed shearing at 45-55° C. and 12000-18000 r / min for 5-10 min.
[0019] Preferably, the high-pressure homogenization condition is: high-pressure homogenization at 45-55 MPa for 1-3 times.
[0020] Preferably, the lysolecithin can be commercially available lysolecithin or can be prepared by the following method.
[0021] Preferably, the lysolecithin is prepared by the following method:
[0022] Tea polyphenols and Tween 80 are added to a phosphate buffer solution, heated and stirred, and then soybean lecithin and glycyrrhizic acid are added and ultrasonicated to obtain a substrate emulsion; phospholipase is added to the substrate emulsion for enzymolysis, and then calcium chloride and glycyrrhizic acid are added to continue the enzymolysis, after the end of the enzyme is inactivated, disodium ethylenediaminetetraacetic acid is added and mixed evenly, centrifuged, the supernatant is collected, acetone is added to the supernatant and mixed evenly, after standing and stratifying, the precipitate is collected and freeze-dried to obtain lysolecithin.
[0023] The preparation of the above-mentioned lysolecithin adopts phospholipase directed enzymolysis technology, and glycyrrhizic acid and tea polyphenols are used to synergistically regulate enzyme activity and reaction microenvironment, thereby improving product uniformity. As a natural antioxidant, tea polyphenols form composite micelles with Tween 80 during ultrasonic dispersion, effectively inhibiting the oxidative degradation of soybean lecithin and ensuring the structural integrity of the substrate. Glycyrrhizic acid can not only stabilize the enzyme active center through hydrogen bonds, optimize enzymolysis conditions, and improve substrate affinity, but also help to enhance the thermal stability and chemical stability of the enzymolysis product. Glycyrrhizic acid and tea polyphenols form an intermolecular hydrogen bond network, and construct a pH buffer layer on the surface of the enzymolysis product, so that the lysolecithin maintains stable performance in the gastric acid environment. Phospholipase specifically hydrolyzes the sn-2 ester bond of lecithin under Ca²⁺ activation to generate high-purity lysolecithin, whose molecular structure exposes more hydrophilic polar heads and increases the HLB value. This structural optimization gives it a stronger water-in-oil emulsification ability and reduces interfacial tension. In addition, disodium ethylenediaminetetraacetic acid chelates metal ions to block the oxidation chain reaction, and acetone precipitation removes unreacted hydrophobic components. The final product can form stable chylomicrons with an increased specific surface area, which significantly improves the contact efficiency of lipase.
[0024] Preferably, the weight ratio of tea polyphenols, Tween 80, glycyrrhizic acid and soybean lecithin in the substrate emulsion is (0.2-0.5):(0.04-0.06):(0.3-0.5):(50-70).
[0025] Preferably, the weight ratio of the phospholipase to soybean lecithin is (0.4-0.6):(50-70).
[0026] Preferably, during the enzymatic hydrolysis process, the weight ratio of calcium chloride, glycyrrhizic acid and phospholipase is (0.1-0.2):(0.05-0.15):(0.4-0.6).
[0027] Preferably, the weight ratio of disodium edetate to soybean lecithin is (0.05-0.1):(50-70).
[0028] Preferably, the lysolecithin is prepared by the following method:
[0029] 0.2-0.5 parts by weight of tea polyphenols and 0.04-0.06 parts by weight of Tween 80 are added to 100-150 parts by weight of phosphate buffer, stirred at 40-50° C. and 200-400 r / min for 10-20 min, then 50-70 parts by weight of soybean lecithin and 0.3-0.5 parts by weight of glycyrrhizic acid are added and ultrasonicated for 15-30 min to obtain a substrate emulsion; 0.4-0.6 parts by weight of phospholipase are added to the substrate emulsion, and stirred at 45-50° C. and 45-50° C. , enzymolysis at 100-200r / min for 20-40min, then raise the temperature to 50-55°C, add 0.1-0.2 weight parts of calcium chloride and 0.05-0.15 weight parts of glycyrrhizic acid and continue enzymolysis for 120-160min, inactivate the enzyme after completion, add 0.05-0.1 weight parts of disodium ethylenediaminetetraacetate and mix evenly, centrifuge, collect the supernatant, add acetone to the supernatant and mix evenly, let stand for stratification, collect the precipitate, and freeze-dry to obtain lysolecithin.
[0030] Preferably, the frequency of the ultrasound is 25-40kHz and the power is 100-300W.
[0031] Preferably, the enzyme inactivation temperature is 80-90°C and the time is 10-20 min.
[0032] Preferably, the amount of acetone added is 2-4 times the volume of the supernatant.
[0033] Preferably, the pH value of the phosphate buffer is 6.5-7.5 and the concentration is 0.1-0.3 mol / L.
[0034] Preferably, the phospholipase is at least one of phospholipase A1 and phospholipase A2.
[0035] Preferably, the phospholipase is phospholipase A2.
[0036] Preferably, the enzyme activity of the phospholipase A2 is 600-1500 U / mg.
[0037] Preferably, the HLB value of lysolecithin is 12-15, the HLB value of polyglycerol fatty acid ester is 2-16, the HLB value of sucrose fatty acid ester is 10-16, and the HLB value of glyceryl monostearate is 3-5.
[0038] The invention also provides a feed emulsifier with high content of lysolecithin, which is prepared by adopting the production method.
[0039] The present invention also provides the use of the above-mentioned high-content lysolecithin feed emulsifier in the preparation of animal feed.
[0040] Beneficial effects of the present invention:
[0041] The present invention provides a method for producing a feed emulsifier with a high content of lysolecithin, by adopting a synergistic effect of specific lysolecithin and sucrose fatty acid ester, taurine, glyceryl monostearate, polyglycerol fatty acid ester, etc., the emulsification performance and emulsification stability of the emulsifier are further improved. The feed emulsifier of the present invention has a high content of lysolecithin, which can significantly improve the digestibility and utilization rate of fat and prevent the occurrence of diarrhea in animals. The present invention also provides the use of the above-mentioned feed emulsifier with a high content of lysolecithin in the preparation of animal feed. DETAILED DESCRIPTION
[0042] The following will be combined with the specific embodiments of the present invention to clearly and completely describe the technical solutions in the embodiments of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. 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.
[0043] Some of the raw materials used in the examples are described below:
[0044] Soybean lecithin, model: PC-60, phosphatidylcholine content: ≥60%, purchased from Zhejiang Ruili Biotechnology Co., Ltd.
[0045] Silicon dioxide, model: AM-SiO2-001-1, gas phase, was purchased from Zhejiang Yamei Nano Technology Co., Ltd.
[0046] Sucrose fatty acid esters, CAS: 37318-31-3, were purchased from Shanghai Titan Technology Co., Ltd.
[0047] Glyceryl monostearate, CAS: 31566-31-1, was purchased from Shanghai Titan Technology Co., Ltd.
[0048] Polyglycerol fatty acid esters, CAS: 67784-82-1, were purchased from Henan Zhengtong Food Technology Co., Ltd.
[0049] Sodium alginate, CAS: 9005-38-3, was purchased from Qingdao Nanshan Biotechnology Co., Ltd.
[0050] Hydroxypropyl-β-cyclodextrin, CAS: 94035-02-6, was purchased from Hubei Dibai Chemical Co., Ltd.
[0051] Example 1
[0052] A method for producing a feed emulsifier with a high content of lysolecithin comprises the following steps:
[0053] S1. Mix 60 parts by weight of lysolecithin, 15 parts by weight of sucrose fatty acid ester, 2 parts by weight of taurine, 5 parts by weight of silicon dioxide and 200 parts by weight of 2wt% sodium alginate aqueous solution, stir at 50°C and 300r / min for 25min to obtain an aqueous phase; mix 10 parts by weight of glyceryl monostearate and 12 parts by weight of polyglycerol fatty acid ester, stir at 60°C and 200r / min for 15min to obtain an oil phase; mix 1 part by weight of ascorbyl glucoside with 50 parts by weight of 10wt% hydroxypropyl-β-cyclodextrin aqueous solution, stir at 55°C and 200r / min for 12h, concentrate under reduced pressure to 20% of the original weight, and freeze-dry to obtain a coated antioxidant;
[0054] S2. Combine 20 parts by weight of the oil phase with 180 parts by weight of the water phase, high-speed shear at 50° C. and 15,000 r / min for 8 min, and then high-pressure homogenize twice at 50 MPa, add 3 parts by weight of the coated antioxidant, stir at 25° C. and 300 r / min for 5 min, spray dry, and pass through an 80-mesh sieve to obtain the feed emulsifier with a high content of lysolecithin.
[0055] The lysolecithin is prepared by the following method:
[0056] 0.35 parts by weight of tea polyphenols and 0.05 parts by weight of Tween 80 are added to 140 parts by weight of phosphate buffer, stirred at 45°C and 300 r / min for 15 minutes, then 60 parts by weight of soybean lecithin and 0.4 parts by weight of glycyrrhizic acid are added and ultrasonicated for 20 minutes, the ultrasonic frequency is 30kHz, and the ultrasonic power is 200W to obtain a substrate emulsion; 0.5 parts by weight of phospholipase A2 is added to the substrate emulsion, enzymolysis is carried out at 50°C and 150 r / min for 30 minutes, then the temperature is raised to 55°C, 0.15 parts by weight of calcium chloride and 0.1 parts by weight of glycyrrhizic acid are added to continue enzymolysis for 150 minutes, after the end, the temperature is raised to 85°C for 15 minutes to inactivate the enzyme, 0.08 parts by weight of disodium ethylenediaminetetraacetate are added, mixed evenly, centrifuged, the supernatant is collected, 3 times the volume of acetone of the supernatant is added to the supernatant, mixed evenly, the precipitate is collected after standing and stratification, and freeze-dried to obtain lysolecithin. Among them, phosphate buffer: pH value is 6.8, concentration is 0.2 mol / L; phospholipase A2: enzyme activity is 1000U / mg.
[0057] Example 2
[0058] A method for producing a feed emulsifier with a high content of lysolecithin comprises the following steps:
[0059] S1. Mix 50 parts by weight of lysolecithin, 10 parts by weight of sucrose fatty acid ester, 1 part by weight of taurine, 3 parts by weight of silicon dioxide and 150 parts by weight of 1wt% sodium alginate aqueous solution, stir at 45°C and 200r / min for 20min to obtain an aqueous phase; mix 7 parts by weight of glyceryl monostearate and 10 parts by weight of polyglycerol fatty acid ester, stir at 58°C and 100r / min for 10min to obtain an oil phase; mix 0.5 parts by weight of ascorbyl glucoside with 40-60 parts by weight of 7wt% hydroxypropyl-β-cyclodextrin aqueous solution, stir at 50°C and 100r / min for 10h, concentrate under reduced pressure to 15% of the original weight, and freeze-dry to obtain a coated antioxidant;
[0060] S2. Combine 15 parts by weight of the oil phase with 150 parts by weight of the water phase, high-speed shear at 45° C. and 12,000 r / min for 10 min, and then high-pressure homogenize at 45 MPa for 3 times, add 2 parts by weight of the coated antioxidant, stir at 23° C. and 200 r / min for 3 min, spray dry, and pass through a 60-mesh sieve to obtain the feed emulsifier with a high content of lysolecithin.
[0061] The lysolecithin is the same as that in Example 1.
[0062] Example 3
[0063] A method for producing a feed emulsifier with a high content of lysolecithin comprises the following steps:
[0064] S1. Mix 70 parts by weight of lysolecithin, 20 parts by weight of sucrose fatty acid ester, 3 parts by weight of taurine, 6 parts by weight of silicon dioxide and 250 parts by weight of 3wt% sodium alginate aqueous solution, stir at 55°C and 400r / min for 30min to obtain an aqueous phase; mix 12 parts by weight of glyceryl monostearate and 15 parts by weight of polyglycerol fatty acid ester, stir at 66°C and 300r / min for 20min to obtain an oil phase; mix 1.5 parts by weight of ascorbyl glucoside and 60 parts by weight of 12wt% hydroxypropyl-β-cyclodextrin aqueous solution, stir at 60°C and 300r / min for 15h, concentrate under reduced pressure to 25% of the original weight, and freeze-dry to obtain a coated antioxidant;
[0065] S2. Combine 25 parts by weight of the oil phase with 200 parts by weight of the water phase, high-speed shear at 55° C. and 18,000 r / min for 5 min, and then high-pressure homogenize once at 55 MPa, add 5 parts by weight of the coated antioxidant, stir at 27° C. and 400 r / min for 7 min, spray dry, and pass through a 100-mesh sieve to obtain the feed emulsifier with a high content of lysolecithin.
[0066] The lysolecithin is the same as that in Example 1.
[0067] Example 4
[0068] A method for producing a feed emulsifier with a high content of lysolecithin comprises the following steps:
[0069] S1. Mix 60 parts by weight of lysolecithin, 15 parts by weight of sucrose fatty acid ester, 2 parts by weight of taurine, 5 parts by weight of silicon dioxide and 200 parts by weight of 2wt% sodium alginate aqueous solution, stir at 50°C and 300r / min for 25min to obtain an aqueous phase; mix 10 parts by weight of glyceryl monostearate and 12 parts by weight of polyglycerol fatty acid ester, stir at 60°C and 200r / min for 15min to obtain an oil phase; mix 1 part by weight of ascorbyl glucoside with 50 parts by weight of 10wt% hydroxypropyl-β-cyclodextrin aqueous solution, stir at 55°C and 200r / min for 12h, concentrate under reduced pressure to 20% of the original weight, and freeze-dry to obtain a coated antioxidant;
[0070] S2. Combine 20 parts by weight of the oil phase with 180 parts by weight of the water phase, high-speed shear at 50° C. and 15,000 r / min for 8 min, and then high-pressure homogenize twice at 50 MPa, add 3 parts by weight of the coated antioxidant, stir at 25° C. and 300 r / min for 5 min, spray dry, and pass through an 80-mesh sieve to obtain the feed emulsifier with a high content of lysolecithin.
[0071] The lysolecithin is prepared by the following method:
[0072] Add 60 parts by weight of soybean lecithin to 140 parts by weight of phosphate buffer and ultrasonicate for 20 minutes, the ultrasonic frequency is 30kHz, the ultrasonic power is 200W, and a substrate liquid is obtained; add 0.5 parts by weight of phospholipase A2 to the substrate liquid, enzymolyze at 50°C and 150r / min for 30 minutes, then heat to 55°C, add 0.15 parts by weight of calcium chloride to continue enzymolysis for 150 minutes, heat to 85°C to kill the enzyme for 15 minutes, add 0.08 parts by weight of disodium ethylenediaminetetraacetate, mix evenly, centrifuge, collect the supernatant, add acetone 3 times the volume of the supernatant to the supernatant, mix evenly, collect the precipitate after standing and stratifying, freeze-dry, and obtain lysolecithin. Wherein, the phosphate buffer: pH value is 6.8, concentration is 0.2mol / L; phospholipase A2: enzyme activity is 1000U / mg.
[0073] Example 5
[0074] A method for producing a feed emulsifier with a high content of lysolecithin comprises the following steps:
[0075] S1. Mix 60 parts by weight of lysolecithin, 15 parts by weight of sucrose fatty acid ester, 2 parts by weight of taurine, 5 parts by weight of silicon dioxide and 200 parts by weight of 2wt% sodium alginate aqueous solution, stir at 50°C and 300r / min for 25min to obtain an aqueous phase; mix 10 parts by weight of glyceryl monostearate and 12 parts by weight of polyglycerol fatty acid ester, stir at 60°C and 200r / min for 15min to obtain an oil phase; mix 1 part by weight of ascorbyl glucoside with 50 parts by weight of 10wt% hydroxypropyl-β-cyclodextrin aqueous solution, stir at 55°C and 200r / min for 12h, concentrate under reduced pressure to 20% of the original weight, and freeze-dry to obtain a coated antioxidant;
[0076] S2. Combine 20 parts by weight of the oil phase with 180 parts by weight of the water phase, high-speed shear at 50° C. and 15,000 r / min for 8 min, and then high-pressure homogenize twice at 50 MPa, add 3 parts by weight of the coated antioxidant, stir at 25° C. and 300 r / min for 5 min, spray dry, and pass through an 80-mesh sieve to obtain the feed emulsifier with a high content of lysolecithin.
[0077] The lysolecithin is prepared by the following method:
[0078] 0.35 parts by weight of tea polyphenols and 0.05 parts by weight of Tween 80 are added to 140 parts by weight of phosphate buffer, stirred at 45°C and 300 r / min for 15 minutes, then 60 parts by weight of soybean lecithin are added and ultrasonicated for 20 minutes, the ultrasonic frequency is 30kHz, and the ultrasonic power is 200W to obtain a substrate emulsion; 0.5 parts by weight of phospholipase A2 is added to the substrate emulsion, enzymolysis is carried out at 50°C and 150 r / min for 30 minutes, then the temperature is raised to 55°C, 0.15 parts by weight of calcium chloride is added to continue enzymolysis for 150 minutes, after the temperature is raised to 85°C for 15 minutes to inactivate the enzyme, 0.08 parts by weight of disodium ethylenediaminetetraacetate is added, mixed evenly, centrifuged, the supernatant is collected, 3 times the volume of acetone of the supernatant is added to the supernatant, mixed evenly, the precipitate is collected after standing and stratification, and freeze-dried to obtain lysolecithin. Among them, phosphate buffer: pH value is 6.8, concentration is 0.2 mol / L; phospholipase A2: enzyme activity is 1000U / mg.
[0079] Example 6
[0080] A method for producing a feed emulsifier with a high content of lysolecithin comprises the following steps:
[0081] S1. Mix 60 parts by weight of lysolecithin, 15 parts by weight of sucrose fatty acid ester, 2 parts by weight of taurine, 5 parts by weight of silicon dioxide and 200 parts by weight of 2wt% sodium alginate aqueous solution, stir at 50°C and 300r / min for 25min to obtain an aqueous phase; mix 10 parts by weight of glyceryl monostearate and 12 parts by weight of polyglycerol fatty acid ester, stir at 60°C and 200r / min for 15min to obtain an oil phase; mix 1 part by weight of ascorbyl glucoside with 50 parts by weight of 10wt% hydroxypropyl-β-cyclodextrin aqueous solution, stir at 55°C and 200r / min for 12h, concentrate under reduced pressure to 20% of the original weight, and freeze-dry to obtain a coated antioxidant;
[0082] S2. Combine 20 parts by weight of the oil phase with 180 parts by weight of the water phase, high-speed shear at 50° C. and 15,000 r / min for 8 min, and then high-pressure homogenize twice at 50 MPa, add 3 parts by weight of the coated antioxidant, stir at 25° C. and 300 r / min for 5 min, spray dry, and pass through an 80-mesh sieve to obtain the feed emulsifier with a high content of lysolecithin.
[0083] The lysolecithin is prepared by the following method:
[0084] Add 60 parts by weight of soybean lecithin and 0.4 parts by weight of glycyrrhizic acid to 140 parts by weight of phosphate buffer, and ultrasonicate for 20 minutes, with an ultrasonic frequency of 30kHz and an ultrasonic power of 200W to obtain a substrate liquid; add 0.5 parts by weight of phospholipase A2 to the substrate liquid, enzymolyze for 30 minutes at 50°C and 150r / min, then heat to 55°C, add 0.15 parts by weight of calcium chloride and 0.1 parts by weight of glycyrrhizic acid to continue enzymolysis for 150 minutes, heat to 85°C to kill the enzyme for 15 minutes, add 0.08 parts by weight of disodium ethylenediaminetetraacetate, mix evenly, centrifuge, collect the supernatant, add acetone 3 times the volume of the supernatant to the supernatant, mix evenly, collect the precipitate after standing and stratifying, and freeze-dry to obtain lysolecithin. Wherein, the phosphate buffer: pH value is 6.8, concentration is 0.2mol / L; phospholipase A2: enzyme activity is 1000U / mg.
[0085] Example 7
[0086] A method for producing a feed emulsifier with a high content of lysolecithin comprises the following steps:
[0087] S1, 60 parts by weight of lysolecithin, 15 parts by weight of sucrose fatty acid ester, 2 parts by weight of taurine, 5 parts by weight of silicon dioxide and 200 parts by weight of 2wt% sodium alginate aqueous solution were mixed, and stirred at 50°C and 300 r / min for 25 min to obtain an aqueous phase; 10 parts by weight of glyceryl monostearate and 12 parts by weight of polyglycerol fatty acid ester were mixed, and stirred at 60°C and 200 r / min for 15 min to obtain an oil phase;
[0088] S2. Combine 20 parts by weight of the oil phase with 180 parts by weight of the water phase, high-speed shear at 50° C. and 15,000 r / min for 8 min, and then high-pressure homogenize twice at 50 MPa, add 0.5 parts by weight of ascorbyl glucoside, stir at 25° C. and 300 r / min for 5 min, spray dry, and pass through an 80-mesh sieve to obtain the feed emulsifier with a high content of lysolecithin.
[0089] The lysolecithin is the same as that in Example 1.
[0090] Example 8
[0091] A method for producing a feed emulsifier with a high content of lysolecithin comprises the following steps:
[0092] S1. Mix 75 parts by weight of lysolecithin, 2 parts by weight of taurine, 5 parts by weight of silicon dioxide and 200 parts by weight of 2wt% sodium alginate aqueous solution, stir at 50°C and 300r / min for 25min to obtain an aqueous phase; heat monostearate to 60°C to melt to obtain an oil phase; mix 1 part by weight of ascorbyl glucoside with 50 parts by weight of 10wt% hydroxypropyl-β-cyclodextrin aqueous solution, stir at 55°C and 200r / min for 12h, concentrate under reduced pressure to 20% of the original weight, and freeze-dry to obtain a coated antioxidant;
[0093] S2. Combine 20 parts by weight of the oil phase with 180 parts by weight of the water phase, high-speed shear at 50° C. and 15,000 r / min for 8 min, and then high-pressure homogenize twice at 50 MPa, add 3 parts by weight of the coated antioxidant, stir at 25° C. and 300 r / min for 5 min, spray dry, and pass through an 80-mesh sieve to obtain the feed emulsifier with a high content of lysolecithin.
[0094] The lysolecithin is the same as that in Example 1.
[0095] Test Example 1
[0096] Take the feed emulsifier prepared in Example 1 as an example to determine the test concentration of the feed emulsifier. Prepare the following feed emulsifier aqueous solutions of different concentrations: 0.025wt%, 0.05wt%, 0.1wt%, 0.2wt%, 0.4wt%, 0.8wt%. Take 20mL of the feed emulsifier aqueous solution and 10mL of soybean oil (acid value ≤ 0.5mg KOH / g) and add them to a graduated test tube, disperse at high speed at 12000r / min for 5min, then stand at room temperature for 24h, and measure the percentage of the emulsified layer volume to the total volume, which is the emulsification index E. 24 . E 24 The larger the value, the better the emulsification ability. In order to eliminate the influence of random errors, the test was set up in 10 parallel groups and the average value was calculated. The results are shown in Table 1.
[0097] Table 1. Emulsification index of feed emulsifiers at different concentrations
[0098] Concentration / wt% 0.025 0.05 0.1 0.2 0.4 0.8 Emulsification index / % 11.2 24.6 56.5 83.7 100 100
[0099] As can be seen from Table 1, the emulsification index of the feed emulsifier gradually increases with the increase of concentration. When the concentration is 0.4wt%, its emulsification index reaches 100%, and the emulsion does not separate within 24h. Therefore, the test concentration of the subsequent emulsifier is determined to be 0.4wt%.
[0100] Test Example 2
[0101] Emulsifying ability: The feed emulsifier prepared in Examples 1-8 was prepared into a feed emulsifier aqueous solution with a concentration of 0.4wt%. Emulsification index determination method: 20mL of the above feed emulsifier aqueous solution and 10mL of soybean oil (acid value ≤ 0.5mgKOH / g) were added to a graduated test tube, dispersed at a high speed of 12000r / min for 5min, and then allowed to stand at room temperature for 24h. The percentage of the emulsified layer volume to the total volume was measured as the emulsification index E. 24 In order to eliminate the influence of random errors, the experiment was set up in 10 parallel groups and the average value was calculated. The results are shown in Table 2.
[0102] Acid resistance stability: The feed emulsifier prepared in Examples 1-8 was formulated into a feed emulsifier aqueous solution with a concentration of 0.4wt%, and the pH value of the feed emulsifier aqueous solution was adjusted to 3.5 using hydrochloric acid. The emulsification index was determined according to the above method. In order to eliminate the influence of random errors, 10 parallel groups were set up in the test and the average value was calculated. The results are shown in Table 2.
[0103] High temperature stability: The feed emulsifier prepared in Examples 1-8 was formulated into a feed emulsifier aqueous solution with a concentration of 0.4wt%, kept at a constant temperature of 80°C for 90 minutes, and then cooled to room temperature for 24 hours. The emulsification index was determined according to the above method. In order to eliminate the influence of random errors, 10 parallel groups were set up in the test and the average value was calculated. The results are shown in Table 2.
[0104] Table 2. Emulsification capacity and stability of feed emulsifiers
[0105]
[0106] As can be seen from Table 2, the feed emulsifiers prepared in Examples 1-3 have the best emulsifying ability and acid and high temperature stability. Their excellent emulsifying effect and high stability provide favorable guarantees for the subsequent application of feed emulsifiers in emulsification and processing of feed, thereby effectively improving the digestibility and utilization rate of oil. Compared with Example 1, the feed emulsifiers prepared in Examples 4-6 do not use lysolecithin prepared by a specific method, Example 7 does not use coated antioxidants, and Example 8 does not use sucrose fatty acid esters and polyglycerol fatty acid esters to synergize with other components, resulting in a certain degree of decline in the emulsifying ability and acid resistance, high temperature stability and other comprehensive properties of the feed emulsifier, further proving the importance of the technical solutions defined in Examples 1-3 of the present invention for achieving the above-mentioned technical effects of the present invention.
[0107] The preferred specific embodiments of the present invention are described in detail above. It should be understood that a person skilled in the art can make many modifications and changes based on the concept of the present invention without creative work. Therefore, any technical solution that can be obtained by a person skilled in the art through logical analysis, reasoning or limited experiments based on the concept of the present invention on the basis of the prior art should be within the scope of protection determined by the claims.
Claims
1. A method for producing a feed emulsifier containing high content of lysolecithin, characterized in that: The following steps are involved: S1. Mix 50-70 parts by weight of lysolecithin, 10-20 parts by weight of sucrose fatty acid ester, 1-3 parts by weight of taurine, 3-6 parts by weight of silicon dioxide and 150-250 parts by weight of sodium alginate aqueous solution, heat and stir to obtain a water phase; mix 7-12 parts by weight of glyceryl monostearate and 10-15 parts by weight of polyglycerol fatty acid ester, heat and stir to obtain an oil phase; S2. 15-25 parts by weight of the oil phase and 150-200 parts by weight of the water phase are combined, and the mixture is subjected to high-speed shearing and high-pressure homogenization in sequence. Then, 2-5 parts by weight of the coated antioxidant is added, stirred, spray-dried, and sieved to obtain the feed emulsifier containing a high content of lysolecithin.
2. The method for producing a feed emulsifier containing high content of lysolecithin according to claim 1, characterized in that: The lysolecithin is prepared by the following method: Tea polyphenols and Tween 80 are added to a phosphate buffer solution, heated and stirred, and then soybean lecithin and glycyrrhizic acid are added and ultrasonicated to obtain a substrate emulsion; phospholipase is added to the substrate emulsion for enzymolysis, and then calcium chloride and glycyrrhizic acid are added to continue the enzymolysis, after the end of the enzyme is inactivated, disodium ethylenediaminetetraacetic acid is added and mixed evenly, centrifuged, the supernatant is collected, acetone is added to the supernatant and mixed evenly, after standing and stratifying, the precipitate is collected and freeze-dried to obtain lysolecithin.
3. The method for producing a feed emulsifier containing high content of lysolecithin according to claim 2, characterized in that: In the substrate emulsion, the weight ratio of tea polyphenols, Tween 80, glycyrrhizic acid and soybean lecithin is (0.2-0.5):(0.04-0.06):(0.3-0.5):(50-70); the weight ratio of phospholipase and soybean lecithin is (0.4-0.6):(50-70).
4. The method for producing a feed emulsifier containing high content of lysolecithin according to claim 2, characterized in that: During the enzymatic hydrolysis process, the weight ratio of calcium chloride, glycyrrhizic acid and phospholipase is (0.1-0.2):(0.05-0.15):(0.4-0.6); the weight ratio of disodium ethylenediaminetetraacetic acid and soybean lecithin is (0.05-0.1):(50-70).
5. The method for producing a feed emulsifier containing high content of lysolecithin according to claim 2, characterized in that: The phospholipase is at least one of phospholipase A1 and phospholipase A2.
6. The method for producing a feed emulsifier containing high content of lysolecithin according to claim 1, characterized in that: The coated antioxidant is prepared by the following method: 0.5-1.5 parts by weight of ascorbyl glucoside and 40-60 parts by weight of hydroxypropyl-β-cyclodextrin aqueous solution are mixed, heated and stirred, concentrated under reduced pressure, and freeze-dried to obtain a coated antioxidant.
7. The method for producing a feed emulsifier containing high content of lysolecithin according to claim 1, characterized in that: The rotation speed of the high-speed shearing is 12000-18000 r / min.
8. The method for producing a feed emulsifier containing a high content of lysolecithin according to claim 1, wherein the pressure of the high-pressure homogenization is 45-55 MPa.
9. A feed emulsifier containing high content of lysolecithin, characterized in that: Prepared according to the production method according to any one of claims 1 to 8.
10. Use of the feed emulsifier containing a high content of lysolecithin according to claim 9 in the preparation of animal feed.
Citation Information
Patent Citations
Preparation method of lysophospholipids
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Feed lysolecithin and preparation method thereof, feed emulsifier and preparation method thereof
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