An oil-in-water emulsion system, method of manufacture and use
Patent Information
- Application Number
- CN202510486400.6
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2025-04-17
- Publication Date
- 2026-08-18
- Estimated Expiration
- 2045-04-17
AI Technical Summary
[0010]对于仔猪用的脂肪酸油脂来说,其配方复杂,普通的乳化体系难于满足应用要求
[0030]本发明使用特定比例和用量吐温60和单甘脂,可以使乳液微胶囊的粒径维持在250nm以下,优选地,维持在200nm以下;
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Abstract
Description
Technical Field
[0001] This invention relates to the field of feed, and more particularly to an oil-in-water emulsion system, its preparation method, and its uses. Background Technology
[0002] Fatty acids are the main components of oils and fats. Animal livers and adipose tissues consume a significant amount of energy and experience substantial heat loss during fat synthesis. However, adding oils and fats to piglet diets can reduce the synthesis of endogenous fatty acids, decrease energy consumption, improve feed conversion ratio, and increase economic benefits. Furthermore, adding fatty acids to piglet diets can reduce diarrhea and mortality in piglets. However, because different fatty acids have different effects on piglets and vary in absorption and metabolism, it is crucial to rationally combine different oils and fats according to their fatty acid composition and content to achieve a balance of fatty acids, which is more important for promoting piglet growth.
[0003] However, directly adding oil to feed can easily cause feed clumping and poor mixing uniformity. Furthermore, the unsaturated fatty acids in oil are easily oxidized and deteriorated by various environmental factors. Therefore, special oil processing techniques are required when adding oil. Common oil processing methods are divided into adsorption and coating types. Adsorption processing involves adding emulsifiers to the oil beforehand, stirring evenly, and then spraying the oil onto a carrier before mixing the carrier with the feed. This method is widely used due to its low production cost and suitability for large-scale feed mills. However, the disadvantages of adsorption processing are that the oil is prone to clumping and oxidation, and the degree of oil adsorption is not high. Emulsion coating is a method of coating oil, with advantages such as high viscosity and good stability. Especially in recent years, nanoemulsions have emerged, which not only retain the characteristics of traditional emulsions but also have higher stability and dispersibility coefficients, and can improve the bioavailability of lipophilic compounds, promoting the absorption of oil by animals. This is a promising processing method. However, oil processing involves many variables, and many factors can affect the quality of nanoemulsions, including the selection of emulsifiers, the amount of emulsifier added, homogenization methods, and process parameters.
[0004] Publication number CN117617366A, entitled "Feed Fatty Acid Composition and Its Application in Poultry Production," discloses the following fatty acid composition: it comprises short-chain fatty acids, medium-chain fatty acids, and long-chain fatty acids, wherein short-chain fatty acids account for 9.9%, medium-chain fatty acids account for 3.22%, and long-chain fatty acids account for 86.66%; saturated fatty acids account for 32.91%, and unsaturated fatty acids account for 66.87%; ω-3 fatty acids account for 4.85%, and ω-6 fatty acids account for 36.28%; the emulsifiers are: sodium citrate 0.5% and mono- and diglycerides 1%; it can form a stable emulsion system.
[0005] Publication No. CN111317067A discloses an emulsified nano-fat powder, its preparation method, and its application. The disclosure specifies that the fat powder contains a combination of unsaturated and saturated fatty acids. Preferably, in the mixed fatty acids, Ω6:Ω3 = (3-4):1. Preferably, the mass ratio of the unsaturated fatty acids to the saturated fatty acids is (1.5-2.8):1. Preferably, the degree of unsaturation of the unsaturated fatty acids is 1-3. Preferably, the unsaturated fatty acids are selected from any one or a combination of at least two of oleic acid, linoleic acid, linolenic acid, palmitoleic acid, arachidonic acid, DHA, eicosapentaenoic acid, or eicosapentaenoic acid. Preferably, the saturated fatty acids are selected from any one or a combination of at least two of caprylic acid, capric acid, lauric acid, myristic acid, palmitic acid, stearic acid, or arachidic acid.
[0006] The emulsifier used is any one or a combination of at least two of lysophosphatidylcholine, sucrose ester, or monoglyceride.
[0007] Publication No. CN107296152A discloses an emulsion composition containing 25-hydroxyvitamin D3 and its preparation method. The emulsion composition contains 25-hydroxyvitamin D3; the dispersed phase oil solvent is one or more of medium-chain triglycerides, glyceryl diacetate, glyceryl triacetate, corn oil, sesame oil, soybean oil, almond oil, peanut oil, peach kernel oil, rapeseed oil, cottonseed oil, sunflower seed oil, castor oil, olive oil, hydrogenated castor oil, and coconut oil; the lipophilic emulsifier is one or more of glyceryl monolinoleate, ethylene glycol monostearate, ethylene glycol monooleate, glyceryl tristearate, glyceryl monostearate, and caprylic / capric triglyceride; the hydrophilic emulsifier includes one or more of Tween-60, Tween-20, Tween-80, sodium lauryl sulfate, potassium lauryl sulfate, and isopropanolamide laurate.
[0008] The embodiments further describe the oil phase as medium-chain triglycerides; the emulsifier is a mixture of monolinoleic acid glycerides and Tween-60 in a weight ratio of approximately 1:2. Its total amount in the formulation is 6.95 wt%.
[0009] The experimental results showed that the product was stable after 90 days of storage under accelerated conditions of 25°C and 60% RH.
[0010] For fatty acid oils used in piglets, the formulation is complex, and ordinary emulsification systems are difficult to meet the application requirements.
[0011] The technical problem this case addresses is: how to better emulsify specific fatty acid oil systems. Summary of the Invention
[0012] The purpose of this invention is to provide an oil-in-water emulsion system that uses a specific ratio and amount of Tween 60 and monoglycerides to maintain the particle size of the emulsion microcapsules below 250 nm, preferably below 200 nm.
[0013] In addition, the present invention also provides a method for preparing the oil-in-water emulsion system and its applications.
[0014] The specific solution of the present invention is as follows:
[0015] An oil-in-water emulsion system, comprising an aqueous phase, an emulsifier, and a balanced oil encapsulated by the emulsifier;
[0016] The amount of the emulsifier used is 2-6 wt%;
[0017] The emulsifier consists of Tween 60 and glyceryl monooleate;
[0018] The weight ratio of unsaturated fatty acids to saturated fatty acids in the balanced oil is greater than 1.5:1; the weight ratio of n-6 fatty acids to n-3 fatty acids is 5 to 10:1.
[0019] In the above-mentioned oil-in-water emulsion system, the amount of the equilibrium oil is 31-33 wt%.
[0020] In the above-mentioned oil-in-water emulsion system, the weight ratio of Tween 60 to glyceryl monooleate is 0.8–1.2:0.8–1.2.
[0021] In the above-mentioned oil-in-water emulsion system, the formulation of the equilibrium oil is as follows:
[0022] The oil contains 10 wt% coconut oil, 2 wt% flaxseed oil, 8 wt% palm oil, 10 wt% rice bran oil, 65 wt% soybean oil, and 5 wt% salmon oil. The weight ratio of unsaturated fatty acids to saturated fatty acids in this balanced oil is greater than 1.5:1; the weight ratio of n-6 fatty acids to n-3 fatty acids is 6:1.
[0023] In the above-mentioned oil-in-water emulsion system, the particle size of the emulsion microcapsules in the oil-in-water emulsion system is 190-250 nm.
[0024] Meanwhile, the present invention also discloses a method for preparing an oil-in-water emulsion system as described above, wherein the method specifically comprises: mixing water, emulsifier, and equilibrium oil, and emulsifying for a period of time under ultrasonic assistance.
[0025] In the above preparation method, the power of the ultrasound is 300-900W.
[0026] In the above preparation method, the ultrasound time is 20 to 60 minutes.
[0027] In the above preparation method, the ultrasonic power is 500-600W and the ultrasonic time is 40-45min.
[0028] Finally, the present invention also discloses the use of oil-in-water emulsion systems as described above in the preparation of feed.
[0029] The beneficial effects of this application are:
[0030] The present invention uses a specific ratio and amount of Tween 60 and monoglycerides to maintain the particle size of emulsion microcapsules below 250 nm, preferably below 200 nm;
[0031] By combining the emulsification system of this invention with the specific advantages of balanced oil in improving the intestinal health and growth of piglets, the nano-sized emulsion can encapsulate the oil, making it more evenly distributed in the piglet feed and reducing the risk of oil oxidation; the smaller particle size of the emulsion can distribute the oil more evenly, enabling it to be absorbed by the piglet intestine more quickly and efficiently, resulting in excellent piglet growth. Detailed Implementation
[0032] The present invention will now be clearly and completely described in conjunction with embodiments thereof. It should be noted that, unless specific conditions are specified in the embodiments, conventional conditions or conditions recommended by the manufacturer shall apply. Reagents or instruments whose manufacturers are not specified are all commercially available conventional products.
[0033] Part 1: The Influence of Different Emulsification Formulas and Processes on the Emulsification Effect of the Same Balanced Oil
[0034] The formula for the balancing oil discussed in this section is as follows:
[0035] Coconut oil 10wt%, flaxseed oil 2wt%, palm oil 8wt%, rice bran oil 10wt%, soybean oil 65wt%, salmon oil 5wt%.
[0036] The emulsion preparation method discussed in this section is as follows:
[0037] Water, balance oil, and emulsifier are mixed in a ratio of 63-65:31-33:2-6, and the above formula is prepared into a nanoemulsion under the set ultrasonic power and duration conditions.
[0038] The relevant experimental conditions are shown in Table 1 below;
[0039] Table 1 Formula and Process Table
[0040]
[0041]
[0042]
[0043] Conclusions and Analysis:
[0044] Based on the experimental results of Examples 1 to 22, it is predicted that the total amount of emulsifier is limited to 5%, the ultrasonic power is between 500 and 600 W, and the ultrasonic time is more than 40 min but less than 60 min, which may produce better results.
[0045] The experimental data were used to perform a three-factor regression analysis on the average particle size of the emulsion using the Design Expert model equation. The multiple quadratic regression model equation for the average particle size of the emulsion (X) with emulsifier dosage (A), ultrasonic power (B), and ultrasonic time (C) is as follows:
[0046] Average particle size (X) = 215.92 - 25.6A + 0.31B - 0.4C - 3.95AB + 0.33AC + 0.83BC - 1.33A 2 +0.37B 2 +1.88C 2
[0047] The multiple quadratic regression model equation for the emulsion PDI (Y) in relation to emulsifier dosage (A), ultrasonic power (B), and ultrasonic time (C) is as follows:
[0048] PDI(Y)=0.26-0.073A-0.015B–8.125×10 -3 C + 0.031AB + 1.5 × 10 -3 AC – 9.75 × 10 - 3 BC
[0049] +9.075×10 -3 A 2 +5.825B 2 +0.018C 2
[0050] The optimal results predicted by the Design Expert model equations are: emulsifier dosage 6wt%, ultrasonic power 541.15W, and ultrasonic time 42.24min.
[0051] After repeated experiments and verifications, the optimal formula and process for preparing balanced oil nanoemulsions by ultrasonic disruption were determined to be: Tween 60 + glyceryl monooleate (1:1) compound emulsifier can reduce the average particle size and PDI of the emulsion. The optimal ultrasonic parameters are 5% compound emulsifier dosage, 540W ultrasonic power and 42min ultrasonic time.
[0052] Part Two: The Effect of the Ratio of Tween 60 and Glyceryl Monooleate on the Emulsification of Balanced Oils
[0053] The adaptability of the balanced oil of the present invention to HLB was studied by adjusting the weight ratio of Tween 60 and glyceryl monooleate to 1:4, 1:2, 2:1, and 4:1.
[0054] The process parameters are as described in Part 1: emulsifier dosage is 5wt%, ultrasonic power is 540W, and time is 42min.
[0055] The balance oil formula is the same as in Part 1;
[0056] Table 2 Formula and Process Table
[0057] Example 24 1 / 4 214.33±1.28 0.317±0.020 Example 25 1 / 2 200.07±0.60 0.280±0.015 Example 26 2 / 1 205.66±1.28 0.237±0.0045 Example 27 4 / 1 201.90±1.30 0.275±0.007
[0058] Results analysis: As can be seen from Examples 23 to 27, after fixing the dosage, emulsification time and ultrasonic power, Tween 60 and glyceryl monooleate at a ratio of 1:1 showed excellent effects.
[0059] Part Three: The Effect of the Same Emulsification on the Emulsification of Different Balance Oils
[0060] This section selects five different formulations of balancing oils: balancing oil 1, balancing oil 2, balancing oil 3, balancing oil 4, and balancing oil 5. Balancing oil 1 is the balancing oil in the first section, containing 10% coconut oil, 2% flaxseed oil, 8% palm oil, 10% rice bran oil, 65% soybean oil, and 5% salmon oil.
[0061] The formula for Balanced Oil 2 is: 5% cottonseed oil, 30% palm oil, 10% rice bran oil, and 55% soybean oil;
[0062] The formula for Balance Oil 3 is: 5% cottonseed oil, 20% palm oil, 10% rice bran oil, 10% sesame oil, 50% soybean oil, and 5% salmon oil.
[0063] The formula for Balance Oil 4 is: 15% oat oil, 5% flaxseed oil, 10% rice bran oil, and 70% soybean oil;
[0064] The formula for Balanced Oil 5 is: 5% lard, 15% oat oil, 10% palm oil, and 70% soybean oil.
[0065] All percentages mentioned above are by weight.
[0066] The above-mentioned balance oils 1 to 5 adopt emulsification process parameters as referred to in Part 1, with an emulsifier dosage of 5wt%, ultrasonic power of 540W, and time of 42min. The emulsifiers are Tween 60 and glyceryl monooleate, with a weight ratio of 1:1.
[0067] The results are shown in Table 3 below;
[0068] Table 3 Formula and Process Table
[0069] Example 28 Balance oil 2 218.69±2.966 0.244±0.003 Example 29 Balance oil 3 206.32±2.436 0.267±0.005 Example 30 Balance oil 4 237.312±2.204 0.364±0.010 Example 31 Balance oil 5 243.279±2.786 0.306±0.006
[0070] Conclusions and Analysis:
[0071] The test results above show that different balance oils are well suited to the emulsification system of this invention, with small particle size and suitable PDI.
[0072] As can be seen from Examples 28 to 31 and Example 23, the process of the present invention has the most significant effect on the balance oil 1, indicating that the process and emulsifier ratio of the present invention have a more obvious adaptability to the balance oil 1 selected in the present invention.
[0073] Part Four: Aquaculture Experiment
[0074] A piglet rearing experiment was conducted using samples with a particle size of less than 200 nm. The rearing process was carried out according to the daily rearing standards of the farm to verify the impact of similar emulsification effects on the rearing results.
[0075] A total of 320 healthy 35-day-old Duroc × Landrace × Large White crossbred piglets (8.45±0.22 kg) were selected for the experiment and randomly divided into 8 treatment groups according to similar weight. Each group had 4 replicates, with 10 piglets per replicate, and the experimental period was 28 days. Balanced oil was added to the diet at 2 wt%.
[0076] The samples used in this section are Example 1, Example 5, Example 10, Example 11, Example 16, Example 18, Example 21, and Example 23.
[0077] The breeding results are as follows:
[0078] Table 4 Piglet Production Performance
[0079]
[0080]
[0081] Results Analysis: The above results show a clear positive correlation between emulsion particle size and feed conversion ratio. When the emulsion particle size is below 200 nm, it can achieve excellent feed conversion ratio results. We believe the reason for this result is as follows:
[0082] On the one hand, the various oils in balanced oils can effectively improve weaning stress and gut health in piglets, thereby enhancing breeding outcomes. For example, palm oil provides the necessary short-chain fatty acids, while coconut oil contains over 60% medium-chain fatty acids. Medium-chain fatty acids can regulate lipid absorption and metabolism in piglets and improve their disease resistance. Furthermore, the n-3 fatty acids abundant in fish oil can promote glucose utilization in piglets, thus promoting growth and alleviating weaning stress.
[0083] On the one hand, nano-sized emulsions can encapsulate oils, making them more evenly distributed in piglet feed and reducing the risk of oil oxidation; smaller particle size emulsions can distribute oils more evenly, enabling them to be absorbed by piglet intestines more quickly and efficiently.
[0084] The combination of the above two points can achieve excellent growth results for piglets.
Claims
1. An oil-in-water emulsion system, characterized in that, Includes the aqueous phase, emulsifier, and balanced oil encapsulated by the emulsifier; The amount of the emulsifier used is 5 wt%; The emulsifier consists of Tween 60 and glyceryl monooleate; The weight ratio of unsaturated fatty acids to saturated fatty acids in the balanced oil is greater than 1.5:1; the weight ratio of n-6 fatty acids to n-3 fatty acids is 5 to 10:
1. The amount of the balance oil used is 31-33 wt%; The weight ratio of Tween 60 to glyceryl monooleate is 1:1; The formula for the balancing oil is as follows: Coconut oil 10wt%, flaxseed oil 2wt%, palm oil 8wt%, rice bran oil 10wt%, soybean oil 65wt%, salmon oil 5wt%. The particle size of the emulsion microcapsules in the oil-in-water emulsion system is maintained below 200 nm; The preparation method of the oil-in-water emulsion system is as follows: mix water, emulsifier, and equilibrium oil, and emulsify for a period of time under ultrasonic assistance; The ultrasonic power is 500-600W, and the ultrasonic time is 40-45 minutes.
2. The use of the oil-in-water emulsion system as described in claim 1 for preparing piglet feed.
Citation Information
Patent Citations
Emulsion composition containing 25-hydroxyvitamin D3 and preparation method thereof
CN107296152A
Emulsified nanometer fatty powder and preparation method and application thereof
CN111317067A
Feed fatty acid composition and application thereof in meat poultry production
CN117617366A
Feed liquid nutrient additive and preparation method and application thereof
CN111449170A
Balancing oil as well as preparation method and application thereof
CN118415277A