Oil-in-water emulsification system, preparation method and application

Abstract

The invention belongs to the field of feed, and discloses an oil-in-water emulsification system which comprises a water phase, an emulsifier and balance oil wrapped by the emulsifier, the dosage of the emulsifier is 2-6 wt%; the emulsifying agent is prepared from Tween 60 and glyceryl monooleate; the weight ratio of unsaturated fatty acid to saturated fatty acid in the balance oil is greater than 1.5: 1; the weight ratio of the n-6 fatty acid to the n-3 fatty acid is (5-10): 1. According to the emulsifying system, Tween 60 and monoglyceride are used in a specific proportion and dosage, so that the particle size of the emulsion microcapsule can be maintained below 250nm, and preferably, the particle size is maintained below 200nm. Meanwhile, the invention also provides a preparation method and application of the oil-in-water emulsification system.

Description

Technical Field

[0001] The present invention relates to the field of feeds, and particularly to an oil-in-water emulsion system, a preparation method and uses thereof. Background Art

[0002] Fatty acids are the main components of oils and fats. A large amount of energy is consumed and a large amount of heat increment occurs during the synthesis of fat in animal livers and adipose tissues. However, adding oils and fats to the diets of piglets can reduce the synthesis of endogenous fatty acids, reduce energy consumption, improve feed conversion rate, and increase the economic benefits of breeding. In addition, adding fatty acids to the diets of piglets can also reduce diarrhea and mortality of piglets. However, since different fatty acids have different effects on piglets and there are differences in absorption and metabolism, it is more important to reasonably match the fatty acid compositions and contents in different oils to achieve the balance of various fatty acids for promoting the growth of piglets.

[0003] However, directly adding oils and fats to feeds is likely to cause feed caking, poor mixing uniformity, and the unsaturated fatty acids in the oils and fats are easily oxidized and deteriorated due to various factors in the environment. Therefore, special oil processing technologies need to be adopted when adding oils and fats. Common oil processing methods are divided into adsorption type and coating type. Adsorption type processing is to add an emulsifier to the oil in advance, stir evenly, and then adsorb the oil on the carrier in the form of spraying, and then mix the carrier with the feed. Because of the low production cost and suitability for large-scale feed mills, it is widely used. However, the disadvantages of adsorption type processing are that the oil is easy to cake and oxidize, and the degree of oil adsorption is not high. Emulsion coating is a method of coating oils and fats. Its advantages are high viscosity and good stability. Especially the nanoemulsions that have emerged in recent years not only retain the characteristics of traditional emulsions, but also have higher stability and dispersion coefficients, and can improve the bioavailability of lipophilic compounds and promote the absorption of oils and fats by animals. It is a processing method with development prospects. However, the oil processing process is variable, and many factors in the processing will affect the quality of nanoemulsions, including mainly the selection of emulsifiers, the addition amount of emulsifiers, homogenization means and process parameters, etc.

[0004] Publication No. CN117617366A, with the theme of a feed fatty acid composition and its application in the production of meat poultry, discloses the following fatty acid combination: it contains short-chain fatty acids, medium-chain fatty acids and long-chain fatty acids. Among them, the proportion of short-chain fatty acids is 9.9%, the proportion of medium-chain fatty acids is 3.22%, and the proportion of long-chain fatty acids is 86.66%; the proportion of saturated fatty acids is 32.91%, and the proportion of unsaturated fatty acids is 66.87%; the proportion of ω-3 fatty acids is 4.85%, and the proportion of ω-6 fatty acids is 36.28%; the emulsifiers are: 0.5% sodium citrate and 1% mono- and diglycerides; it can form a stable emulsion system.

[0005] Publication No. CN111317067A, with the theme of an emulsified nano-fat powder and its preparation method and application, discloses that the fat powder contains a combination of unsaturated fatty acids 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, eicosatetraenoic 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, with the theme of an emulsion composition containing 25-hydroxyvitamin D3 and its preparation method, discloses an emulsion composition containing 25-hydroxyvitamin D3; the dispersed phase oil phase solvent is one or more of medium-chain triglycerides, glycerol diacetate, glycerol 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, coconut oil; the lipophilic emulsifier is one or more of glyceryl monooleate, ethylene glycol monostearate, ethylene glycol monooleate, glyceryl tristearate, glyceryl monostearate, triglycerol caprylate; the hydrophilic emulsifier includes one or more of Tween-60, Tween-20, Tween-80, sodium dodecyl sulfate, potassium dodecyl sulfate, lauric acid isopropanolamide;

[0008] Its examples further describe that the oil phase is medium-chain triglycerides; the emulsifier is formed by mixing glyceryl monooleate and Tween-60, and their weight ratio is close to 1:2. Its total dosage in the prescription is 6.95wt%.

[0009] The experimental result is: stable after being placed for 90 days under the conditions of accelerated 25°C and 60% RH.

[0010] For the fatty acid oils and fats for piglets, its formula is complex, and ordinary emulsification systems are difficult to meet the application requirements.

[0011] The technical problem solved in this case is: how to better emulsify a specific fatty acid oil and fat system. Summary of the Invention

[0012] The object of the present invention is to provide an oil-in-water emulsion system, which uses Tween 60 and glycerol monostearate in specific proportions and amounts, and can maintain the particle size of the emulsion microcapsules below 250 nm, preferably below 200 nm.

[0013] Meanwhile, the present invention also provides a preparation method and uses of the oil-in-water emulsion system.

[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 is 2-6 wt%;

[0017] The emulsifier consists of Tween 60 and glyceryl monooleate;

[0018] In 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 5-10:1.

[0019] In the above oil-in-water emulsion system, the amount of the balanced oil is 31-33 wt%.

[0020] In the above 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 oil-in-water emulsion system, the formulation of the balanced oil is as follows:

[0022] Coconut oil 10 wt%, linseed oil 2 wt%, palm oil 8 wt%, rice bran oil 10 wt%, soybean oil 65 wt%, salmon oil 5 wt%; 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 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 preparation method of an oil-in-water emulsion system as described above, and the method is specifically as follows: Mix water, an emulsifier, and a balanced oil, and emulsify for a period of time under ultrasonic assistance.

[0025] In the above preparation method, the power of the ultrasonic wave is 300-900 w.

[0026] In the above preparation method, the time of the ultrasonic wave is 20-60 min.

[0027] In the above preparation method, the power of the ultrasonic wave is 500-600 w, and the ultrasonic time is 40-45 min.

[0028] Finally, the present invention also discloses the use of the oil-in-water emulsion system described above to prepare feed.

[0029] The beneficial effects of this application are as follows:

[0030] In the present invention, by using Tween 60 and monoglyceride in specific proportions and dosages, the particle size of the emulsion microcapsules can be maintained below 250 nm, preferably below 200 nm.

[0031] Due to the specific advantages of the emulsification system of the present invention combined with the balanced oil in improving the intestinal health of piglets and enhancing the growth effect, the nanoemulsion can coat the oil to make it more evenly distributed in the piglet diet and reduce the risk of oil oxidation; the emulsion with a smaller particle size can distribute the oil more evenly, enabling it to be absorbed by the piglet intestine faster and more efficiently, achieving a very excellent piglet growth effect. Specific Embodiments

[0032] The present invention will be clearly and completely described below in conjunction with the embodiments of the present invention. In the description of the present invention, it should be noted that for those conditions not specified in the embodiments, they are carried out according to the conventional conditions or the conditions recommended by the manufacturer. For the reagents or instruments whose manufacturers are not specified, they are all conventional products that can be obtained through commercial purchase.

[0033] Part I. Influence of Different Emulsification Formulas and Processes on the Emulsification Effect of the Same Balanced Oil

[0034] The formula of the balanced oil involved in this part is as follows:

[0035] Coconut oil 10 wt%, linseed oil 2 wt%, palm oil 8 wt%, rice bran oil 10 wt%, soybean oil 65 wt%, salmon oil 5 wt%.

[0036] The preparation method of the emulsion involved in this part is as follows:

[0037] Water, balanced oil, and emulsifier are proportioned according to the ratio of 63-65:31-33:2-6, and the above prescription is mixed and prepared into a nanoemulsion under the conditions of the set ultrasonic power and duration.

[0038] The relevant experimental conditions are shown in Table 1 below;

[0039] Table 1 Formulation and Process Table

[0040]

[0041]

[0042]

[0043] Conclusions and analysis:

[0044] Based on the experimental results prediction of Examples 1 to 22, when the total amount of emulsifier is limited to 5%, the ultrasonic power is between 500 and 600 W, and the ultrasonic time exceeds 40 min and is less than 60 min, better results may be obtained.

[0045] The above experimental data were analyzed by regression analysis of the average particle size of the emulsion using the Design Expert model equation with three factors. The multiple quadratic regression model equation for the average particle size of the emulsion (X) with respect to the emulsifier dosage (A), ultrasonic power (B), and ultrasonic time (C) is:

[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) with respect to the emulsifier dosage (A), ultrasonic power (B), and ultrasonic time (C) is:

[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] Through the Design Expert model equation, the optimal results are predicted as: emulsifier dosage 6 wt%, ultrasonic power 541.15 W, and ultrasonic time 42.24 min.

[0051] After repeated experiments and verification, the best formulation and process for preparing balanced oil nanoemulsion by ultrasonic fragmentation method were found: the compound emulsifier of Tween 60 + glycerol monooleate (1:1) can reduce the average particle size and PDI of the emulsion, and the best ultrasonic parameters are 5% compound emulsifier dosage, 540 W ultrasonic power, and 42 min ultrasonic time.

[0052] The influence of the ratio of Tween 60 to glycerol monoleate on the emulsification of balanced oil

[0053] By adjusting the weight ratio of Tween 60 to glycerol monoleate to 1:4, 1:2, 2:1, 4:1, the adaptability of the balanced oil of the present invention to HLB was studied.

[0054] The process parameters refer to the first part, with the emulsifier dosage being 5 wt%, the ultrasonic power being 540 W, and the time being 42 min.

[0055] The balanced oil formula is the same as that in the first part;

[0056] Table 2 Formulation and process table

[0057] Tween 60: Glyceryl Monooleate Emulsion Particle Size / nm PDI 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] Result analysis: As can be seen from Examples 23 to 27, after fixing the dosage, emulsification time and ultrasonic power, Tween 60 and glycerol monoleate showed excellent effects when at a ratio of 1:1.

[0059] Part Three The influence of the same emulsification on different balanced oils

[0060] In this part, 5 balanced oils with different formulations were selected, namely balanced oil 1, balanced oil 2, balanced oil 3, balanced oil 4, and balanced oil 5; among them, balanced oil 1 is the balanced oil in the first part; 10% coconut oil, 2% linseed oil, 8% palm oil, 10% rice bran oil, 65% soybean oil, 5% salmon oil;

[0061] The formula of balanced oil 2 is: 5% cottonseed oil, 30% palm oil, 10% rice bran oil, 55% soybean oil;

[0062] The formula of balanced oil 3 is: 5% cottonseed oil, 20% palm oil, 10% rice bran oil, 10% sesame oil, 50% soybean oil, 5% salmon oil;

[0063] The formula of balanced oil 4 is: 15% oat oil, 5% linseed oil, 10% rice bran oil, 70% soybean oil;

[0064] The formula of balanced oil 5 is: 5% lard, 15% oat oil, 10% palm oil, 70% soybean oil.

[0065] The above percentages are all weight percentages.

[0066] For the above-mentioned balanced oils 1 to 5, the emulsification process parameters refer to the first part, with the emulsifier dosage being 5 wt%, the ultrasonic power being 540 W, the time being 42 min, and the emulsifier being Tween 60 and glycerol monoleate with a weight ratio of 1:1.

[0067] The results are shown in Table 3 below;

[0068] Table 3 Formulation and Process Table

[0069] Balanced Oil Emulsion Particle Size / nm PDI Example 28 Balanced Oil 2 218.69±2.966 0.244±0.003 Example 29 Balanced Oil 3 206.32±2.436 0.267±0.005 Example 30 Balanced Oil 4 237.312±2.204 0.364±0.010 Example 31 Balanced Oil 5 243.279±2.786 0.306±0.006

[0070] Conclusions and Analysis:

[0071] From the above test results, it can be seen that different balance oils can all be well applied to the emulsion system of the present invention, with smaller particle sizes and appropriate PDI values.

[0072] Combining Examples 28 to 31 and Example 23, it can be seen that the process of the present invention has the most significant effect on Balance Oil 1, indicating that the process and emulsifier ratio of the present invention have a more obvious adaptability to the selected Balance Oil 1 of the present invention.

[0073] Part Four: Breeding Experiment

[0074] Samples with particle sizes below 200 nm were used for piglet breeding experiments. The breeding process was carried out according to the daily breeding standards of the farm to verify the impact of similar emulsification effects on breeding results.

[0075] A total of 320 healthy 35-day-old Duroc×Landrace×Yorkshire ternary piglets (8.45±0.22 kg) were selected for the experiment. They were randomly divided into 8 treatment groups according to the principle of similar body weight. Each group had 4 replicates, with 10 piglets in each replicate. The experimental period was 28 days. The balance oil added to the diet was 2 wt%.

[0076] The samples used in this part were Example 1, Example 5, Example 10, Example 11, Example 16, Example 18, Example 21, and Example 23.

[0077] The breeding results were as follows:

[0078] Table 4 Piglet Production Performance

[0079]

[0080]

[0081] Result Analysis: From the above results, it can be seen that there is an obvious positive correlation between the emulsion particle size and the feed-to-meat ratio. When the emulsion particle size is below 200 nm, very excellent feed-to-meat ratio results can be achieved. We believe that the reason for this result is:

[0082] On the one hand, thanks to the oils and fats contained in the balanced oil, it can effectively improve the weaning stress of piglets, improve intestinal health, and thus improve the breeding effect. For example, palm oil can provide the lacking short-chain fatty acids, and coconut oil contains more than 60% medium-chain fatty acids. Medium-chain fatty acids can regulate the absorption and metabolism of lipids in piglets and can improve the disease resistance of piglets. In addition, the n-3 fatty acids rich in fish oil can promote the utilization rate of glucose by piglets to promote the growth of piglets and relieve the weaning stress of piglets.

[0083] On the one hand, the nanoemulsion can coat the oil and fat to make it more evenly distributed in the piglet diet and reduce the risk of oil oxidation; the emulsion with a smaller particle size can distribute the oil more evenly, enabling it to be absorbed by the piglet intestine faster and more efficiently.

[0084] The combination of the above two points can achieve very excellent piglet growth effects.

Claims

1. An oil-in-water emulsion system, characterized in that: It includes a water phase, an emulsifier, and a balanced oil wrapped by the emulsifier; The amount of the emulsifier is 2 to 6 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.

2. The oil-in-water emulsion system according to claim 1, characterized in that The amount of the balancing oil is 31-33 wt %.

3. The oil-in-water emulsion system according to claim 1, characterized in that: The weight ratio of Tween 60 to monoolein is 0.8-1.2:0.8-1.

2.

4. The oil-in-water emulsion system according to claim 1, characterized in that The formula of the balancing oil is: Coconut oil 10wt%, linseed oil 2wt%, palm oil 8wt%, rice bran oil 10wt%, soybean oil 65wt%, salmon oil 5wt%.

5. The oil-in-water emulsion system according to claim 1, characterized in that: The particle size of the emulsion microcapsules in the water-in-oil emulsification system is 190-250 nm.

6. A method for preparing an oil-in-water emulsion system according to any one of claims 1 to 5, characterized in that: The method specifically comprises: mixing water, an emulsifier and a balancing oil, and emulsifying the mixture for a period of time under the assistance of ultrasound.

7. The preparation method according to claim 6, characterized in that: The power of the ultrasound is 300-900w.

8. The preparation method according to claim 6, characterized in that: The ultrasonic time is 20 to 60 minutes.

9. The preparation method according to claim 6, characterized in that: The ultrasonic power is 500-600w, and the ultrasonic time is 40-45min.

10. Use of the oil-in-water emulsification system according to any one of claims 1 to 5 in preparing feed.

Images