An acid-alkali-resistant and salt-resistant heat-stable high-oil-loading emulsion, a preparation method and application thereof

Abstract

The application discloses an acid-alkali-resistant and salt-resistant heat-stable high-oil-loading emulsion and a preparation method and application thereof. The emulsion is composed of oil, a main emulsifier, an auxiliary emulsifier, a stabilizer, an antioxidant and deionized water in a specific proportion. In the preparation process, the emulsion is formed through steps of dispersion, dissolution, stirring, shearing and high-pressure homogenization. The oil loading of the emulsion is up to 40% or more. The obtained emulsion is stable in a pH 3-9 range and in a sodium, potassium, calcium and magnesium ion solution, has excellent physical and chemical stability, can remain uniform and stable even after 20 days of accelerated aging at 57 DEG C, and has a peroxide value of less than 0.13 g / 100 g. The emulsion has the advantages of high oil loading, stable system and wide applicability, is suitable for food fields such as various beverages, oral solutions and dietary supplements, breaks through the limitation of the existing emulsion technology, and provides a new type of efficient and stable emulsion product for the food industry.

Description

Technical Field

[0001] This invention belongs to the field of food emulsion technology, and particularly relates to a heat-stable high oil-carrying emulsion that is resistant to acids, alkalis and salts, its preparation method and application. Background Technology

[0002] In recent years, emulsions have been increasingly widely used in the food industry, offering advantages over other dosage forms in the delivery of polyunsaturated fatty acids and fat-soluble active ingredients. An emulsion is a dispersion system formed by two immiscible liquids, in which the dispersed liquid (dispersed phase) is dispersed as small droplets in a continuous liquid (continuous phase). Traditional emulsions have low physical stability and are prone to demulsification under conditions such as heating, cooling, freezing, drying, extreme pH, and high mineral content, thus limiting their application in food.

[0003] Patent CN101259102 discloses a micron-sized docosahexaenoic acid (DHA) emulsion and its preparation method, but specifies the addition amount in health products and foods as 0.05–2.5%, resulting in a low DHA content in the final product and failing to achieve the desired effect. Patent CN104906074A discloses a method for preparing a stable conjugated linoleic acid (CLA) emulsion, but the emulsion particle size increases significantly after storage at 40°C for 7 days, failing to meet market demands for product stability. Patent CN102939079A discloses a heat-stable oil-in-water emulsion containing oils with polyunsaturated fatty acids, but the formula also contains high levels of sodium chloride and monosaccharides, failing to meet consumers' demand for low-salt and low-sugar diets, thus limiting its application.

[0004] Emulsions are thermodynamically unstable systems, prone to flocculation, coagulation, and Australtic ripening during storage, making them difficult to apply in complex environments. Current patents for food emulsions generally suffer from low oil loading, high emulsifier dosage, and poor stability, failing to meet the broad application requirements of the food industry. Therefore, there is an urgent need for a highly stable, high-oil-loading food emulsion product with broad applicability to meet various application scenarios. Summary of the Invention

[0005] This invention aims to provide a heat-stable, high-oil-loading emulsion resistant to acids, alkalis, and salts, and its preparation method. The emulsion prepared by this invention has an oil loading of over 40%, can withstand high-temperature sterilization at 121°C, can rapidly disperse and dissolve in water without stratification or oil floating, and remains stable in environments with pH 3–9 and in solutions containing sodium, potassium, and calcium ions.

[0006] The first aspect of this invention relates to a high-temperature resistant, acid and alkali resistant, and salt resistant high-oil-carrying emulsion, comprising the following raw materials: oil, primary emulsifier, co-emulsifier, stabilizer, antioxidant, and deionized water. The materials, by weight, comprise: 40-55 parts oil, 0.8-3.0 parts primary emulsifier, 0.8-2.0 parts stabilizer, 0.2-2.0 parts antioxidant, 10-35 parts co-emulsifier, and 12.5-40 parts deionized water.

[0007] For the technical solution described above, preferably, the oil is 40-50 parts, the emulsifier is 12.6-30.0 parts, and the deionized water is 24-38 parts;

[0008] For the technical solution described above, preferably, the oil can be selected from one or more of the following: sunflower seed oil, rapeseed oil, soybean oil, corn oil, flaxseed oil, safflower seed oil, coconut oil, camellia seed oil, milk thistle seed oil, olive oil, palm oil, cottonseed oil, peanut oil, perilla seed oil, evening primrose oil, grapeseed oil, almond oil, walnut oil, castor oil, rice bran oil, tiger nut oil, blueberry seed oil, sacha inchi oil, maple seed oil, avocado oil, fish oil, DHA algal oil, medium-chain triglycerides, conjugated linoleic acid glycerides, and diglyceride oil.

[0009] With respect to the technical solution described above, preferably, the amount of the main emulsifier is adjusted according to the amount of oil, and preferably 2.0 to 6.0% of the weight of the oil.

[0010] For the technical solution described above, preferably, the main emulsifier is a nonionic surfactant, including oil-phase emulsifier and aqueous-phase emulsifier.

[0011] For the technical solution described above, preferably, the oil phase emulsifier is selected from one or more of mono- and diglyceride fatty acid esters, sucrose fatty acid esters with a monoester content of less than 30%, and polyglycerol ricinoleate.

[0012] For the technical solution described above, preferably, the oil phase emulsifier accounts for 0.2 to 1.0% of the weight of the oil, and the weight ratio of the water phase emulsifier to the oil phase emulsifier is (3 to 15):1; preferably, the weight ratio of the water phase emulsifier to the oil phase emulsifier is (5 to 10):1.

[0013] The aqueous emulsifier is selected from one or more of sucrose fatty acid esters and polyoxyethylene sorbitan fatty acid esters; preferably, the aqueous emulsifier is selected from sucrose fatty acid esters, or a combination of sucrose fatty acid esters and polyoxyethylene sorbitan fatty acid esters. Preferably, the total ester content of the sucrose fatty acid ester used is greater than 80%, and the monoester content is greater than 70%.

[0014] For the technical solution described above, the preferred weight ratio of the co-emulsifier to deionized water is (0.8-5.0):3; more preferably, the weight ratio of the co-emulsifier to deionized water is (1-4):3; and even more preferably, it is (1-3.75):3.

[0015] With respect to the above-described technical solution, preferably, the co-emulsifier in the formulation is selected from propylene glycol and glycerol, and the weight ratio of propylene glycol to glycerol is 1:(0.5-5); preferably, the weight ratio of propylene glycol to glycerol is 1:(1-3), and more preferably, the weight ratio of propylene glycol to glycerol is 1:(1-1.6).

[0016] For the technical solution described above, preferably, the stabilizer is a composition of polyglycerol fatty acid ester, vitamin E polydiglycolate succinate, and sorbitol. To meet the requirements of high-temperature resistance and freeze-thaw resistance of the emulsion, the polyglycerol fatty acid ester used must have a degree of polymerization of 6-10 and account for more than 50 wt% of the stabilizer composition; preferably, the polyglycerol fatty acid ester accounts for 60-80 wt% of the stabilizer; more preferably, the degree of polymerization of the polyglycerol fatty acid ester is 8-10. More preferably, the stabilizer is composed of polyglycerol fatty acid ester, vitamin E polydiglycolate succinate, and sorbitol in a weight ratio of (8-12):(1-5):(1-5).

[0017] For the technical solution described above, preferably, the antioxidant includes an aqueous phase antioxidant and an oil phase antioxidant. The aqueous phase antioxidant is selected from one or more of ascorbic acid, sodium ascorbate, and sodium D-isoascorbate. The oil phase antioxidant is selected from one or more of mixed tocopherols, ascorbate palmitate, rosemary extract, tert-butylhydroquinone, and butylated hydroxytoluene.

[0018] Another aspect of the present invention relates to a method for preparing the acid-, alkali-, and salt-resistant, heat-stable, high-oil-load-bearing emulsion, comprising the following steps:

[0019] S1. Weigh deionized water, add aqueous emulsifier, disperse it evenly, heat to dissolve, and after complete dissolution, add co-emulsifier and stir until the main emulsifier and co-emulsifier are fully dissolved and in a uniform state; add stabilizer and stir until completely dissolved, at which point a transparent to semi-transparent aqueous phase is obtained;

[0020] S2. Weigh the oil according to the formula, add the oil phase emulsifier and oil phase antioxidant, dissolve them completely to obtain the oil phase;

[0021] S3. While continuously stirring, slowly add the oil phase to the aqueous phase and stir thoroughly to form a primary emulsion;

[0022] S4. Add an aqueous antioxidant to the primary emulsion and continue stirring until the system is homogeneous. Then, subject the emulsion to high-speed shearing and high-pressure homogenization to prepare an emulsion.

[0023] S5. The emulsion obtained in S4 is sterilized and then aseptically bottled to obtain the finished emulsion.

[0024] For the technical solution described above, preferably, the dissolution temperature of the aqueous emulsifier in S1 is 70-75℃.

[0025] For the technical solution described above, preferably, the dissolution temperature of the oil phase emulsifier and antioxidant in S2 is 50-60°C, and the method can be ultrasonic dissolution.

[0026] For the technical solution described above, preferably, the emulsification temperature in S3 is 50-60°C.

[0027] For the technical solution described above, preferably, in step S4, the aqueous antioxidant needs to be pre-dissolved in water and then added to the primary emulsion, and the emulsion stirring speed is 300-500 rpm.

[0028] For the technical solution described above, preferably, the shearing speed in step S4 is 5000-8000 rpm and the shearing time is 3-5 minutes.

[0029] For the technical solution described above, preferably, the homogenization pressure in step S4 is 40-60 MPa, and the number of homogenization steps is 2-3.

[0030] Finally, the present invention also protects the application of the above-mentioned high-temperature resistant, acid and alkali resistant, and salt resistant high-oil-carrying emulsion, the application fields of which include the production of liquid beverages, oral liquids, dietary supplements, etc., wherein liquid beverages include fruit juice beverages, protein beverages, compound functional beverages, etc.

[0031] In addition, this emulsion can also be used in the following specific products:

[0032] Protein and fortified foods: such as sports nutrition drinks, children's nutritional drinks, and foods for special medical purposes; edible oils and condiments: such as salad dressings, mayonnaise, sauces, dairy products; and ice cream, etc.

[0033] The beneficial effects of this invention are:

[0034] 1. The emulsion prepared by this invention has an oil loading of over 40%, good fluidity, and a homogeneous system without stratification or oil drift. The emulsion particle size (D99) is approximately 500–800 nm. The resulting emulsion can withstand high-temperature sterilization at 121°C and remains stable after centrifugation.

[0035] 2. The emulsion prepared by this invention has excellent performance in application. It can be diluted in water at any ratio, remains stable in the pH range of 3 to 9, and remains stable in sodium, potassium, calcium, and magnesium ion solutions.

[0036] 3. The emulsion prepared by this invention also has very good physical and chemical stability. The emulsion remains uniform and stable after being accelerated at 57°C for 20 days, without layering or oil floating, and the peroxide value (based on oil) is less than 0.13 g / 100 g.

[0037] 4. The emulsion prepared by this invention has many advantages such as high oil carrying capacity, stable system, and wide range of applications, and can be widely used in various beverages, oral liquids and dietary supplements and other food fields. Detailed Implementation

[0038] The present invention will be further described below with reference to the embodiments, but it should be understood that the scope of protection of the present invention is not limited to the embodiments.

[0039] In this invention, unless otherwise explicitly stated, percentages and contents are all by mass. Unless otherwise specified, the experimental methods used are conventional methods, and the materials and reagents used are commercially available.

[0040] In this embodiment, the product performance of the samples is evaluated by first taking samples from each sample and dividing them into several parallel samples. In order to ensure the scientificity and credibility of the product performance evaluation, the same number of sub-samples are randomly selected for each product, and the same test conditions and measurement techniques are used for evaluation. The performance is quantified and compared by statistical analysis of the obtained data (calculating the average value).

[0041] Example 1

[0042] Weigh 340g of nonionized water, add 8.5g of sucrose fatty acid ester and 1.5g of polyoxyethylene (20) sorbitan monooleate, stir until evenly dispersed, heat to 75℃, and after fully swelling, add 50g of propylene glycol and 76g of glycerol, dissolve, then add 8g of polyoctaglycerol monooleate, 1g of vitamin E polydiethanol succinate and 1g of sorbitol, stir evenly, this is the aqueous phase.

[0043] Weigh out 160g sunflower seed oil, 150g soybean oil, and 150g corn oil, add 4g rosemary extract and 1.0g mono- and diglyceride fatty acid esters, and dissolve by sonication at 60℃. This is the oil phase.

[0044] The oil phase is slowly added to the aqueous phase while maintaining the temperature at 55°C and the stirring speed at 400 rpm to form a primary emulsion.

[0045] Weigh out 3g of ascorbic acid and 8g of sodium ascorbate, dissolve them in 30g of non-ionized water, and then add them to the above primary emulsion. Stir at 300 rpm, and add water to bring the emulsion mass to 1000g. Shear the emulsion at 5500 rpm for 2 minutes, and homogenize it twice under high pressure at 40MPa to obtain a vegetable oil emulsion, which is then sterilized and stored.

[0046] Example 2

[0047] Weigh 290g of nonionized water, add 9.5g of sucrose fatty acid ester, stir until evenly dispersed, heat to 75℃, and after the sucrose fatty acid ester has fully swollen, add 75g of propylene glycol and 75g of glycerol, dissolve, then add 8g of decaglycerol monodecanoate, 4g of vitamin E polydiethanol succinate, and 3g of sorbitol, and stir evenly. This is the aqueous phase.

[0048] Weigh 500g of medium-chain triglycerides, add 1g of mixed tocopherols and 1.5g of polyglycerol ricinoleate, and sonicate at 50°C to dissolve; this is the oil phase.

[0049] The oil phase is slowly added to the aqueous phase while maintaining the temperature at 60°C and a stirring speed of 500 rpm to form a primary emulsion.

[0050] Weigh 2g of sodium ascorbate and dissolve it in 20g of nonionized water. Then add the solution to the above primary emulsion and stir at 350 rpm. Add water to bring the emulsion mass to 1000g. Shear the emulsion at 5000 rpm for 5 minutes and homogenize it three times under high pressure at 40 MPa to obtain a medium-chain triglyceride emulsion, which is then sterilized and stored.

[0051] Example 3

[0052] Weigh 200g of nonionized water, add 20g of sucrose fatty acid ester, stir until evenly dispersed, heat to 75℃, and after the sucrose fatty acid ester has fully swollen, add 120g of propylene glycol and 180g of glycerol, dissolve, then add 11g of hexaglycerol monolaurate, 3g of vitamin E polydiethanol succinate, and 2g of sorbitol, and stir evenly. This is the aqueous phase.

[0053] Weigh 400g of DHA algal oil, add 1.8g of mixed tocopherols, 0.2g of ascorbate palmitate, and 4.0g of sucrose fatty acid ester (monoester <30%), and dissolve by sonication at 55℃. This is the oil phase.

[0054] The oil phase is slowly added to the aqueous phase while maintaining the temperature at 50°C and the stirring speed at 300 rpm to form a primary emulsion.

[0055] Weigh out 3g of ascorbic acid and 15g of sodium ascorbate, dissolve them in 25g of non-ionized water, and then add them to the above-mentioned primary emulsion. Stir at 350 rpm, and add water to bring the emulsion mass to 1000g. Shear the emulsion at 6000 rpm for 5 minutes, and homogenize it three times under high pressure at 40MPa to obtain DHA emulsion, which is then sterilized and stored.

[0056] Example 4

[0057] Weigh 260g of nonionized water, add 9g of polyoxyethylene (20) sorbitan monooleate, stir until evenly dispersed, heat to 75℃ to fully dissolve, add 37.5g of propylene glycol and 112.5g of glycerol, dissolve, then add 10g of decaglycerol monopalmitate, 5g of vitamin E polydiethanol succinate and 5g of sorbitol, stir evenly, this is the aqueous phase.

[0058] Weigh 500g of conjugated linoleic acid glyceride, add 2g of mixed tocopherols, 0.6g of mono- and diglyceride fatty acid esters and 0.4g of polyglycerol ricinoleate, and dissolve by sonication at 50°C. This is the oil phase.

[0059] The oil phase is slowly added to the aqueous phase while maintaining the temperature at 60°C and a stirring speed of 500 rpm to form a primary emulsion.

[0060] Weigh 10g of sodium ascorbate and dissolve it in 30g of nonionized water. Then add the solution to the primary emulsion and stir at 450 rpm. Add water to bring the emulsion mass to 1000g. Shear the emulsion at 8000 rpm for 3 minutes and homogenize it twice at 60MPa to obtain a conjugated linoleic acid glyceride emulsion. Sterilize and store.

[0061] Example 5

[0062] Weigh 180g of nonionized water, add 8g of sucrose fatty acid ester and 3.2g of polyoxyethylene (20) sorbitan monolaurate, stir until evenly dispersed, heat to 75℃, and after the material is fully dissolved, add 55g of propylene glycol and 275g of glycerol, and after dissolving, add 9g of decaglycerol monooleate, 2g of vitamin E polydiethanol succinate and 1g of sorbitol, and stir evenly. This is the aqueous phase.

[0063] Weigh 420g of refined coconut oil, add 2g of rosemary extract, 1.0g of mono- and diglycerides of fatty acids and 0.4g of sucrose fatty acid ester (monoester <30%), and dissolve by sonication at 55℃. This is the oil phase.

[0064] The oil phase is slowly added to the aqueous phase while maintaining the temperature at 55°C and the stirring speed at 400 rpm to form a primary emulsion.

[0065] Weigh 6g of sodium D-isoascorbate and dissolve it in 30g of nonionized water. Then add it to the above primary emulsion and stir at 300 rpm. Add water to bring the emulsion mass to 1000g. Shear the emulsion at 6000 rpm for 3 minutes and homogenize it three times under high pressure at 50MPa to obtain refined coconut oil emulsion. Sterilize and store.

[0066] Example 6

[0067] Weigh 200g of nonionized water, add 17.45g of sucrose fatty acid ester, stir until evenly dispersed, heat to 70℃, and after the sucrose fatty acid ester has fully swollen, add 79.0g of propylene glycol and 157.9g of glycerol, dissolve, then add 8g of polyoctaglycerol monolaurate, 2g of vitamin E polydiethanol succinate, and 5g of sorbitol, and stir evenly. This is the aqueous phase.

[0068] Weigh 480g of milk thistle seed oil, add 2g of tert-butylhydroquinone, 1g of butylated hydroxytoluene, and 1.75g ​​of sucrose fatty acid ester (monoester <30%), and dissolve by sonication at 50℃. This is the oil phase.

[0069] The oil phase is slowly added to the aqueous phase while maintaining the temperature at 50°C and the stirring speed at 450 rpm to form a primary emulsion.

[0070] Weigh out 3g of ascorbic acid and 6g of sodium D-isoascorbate, dissolve them in 30g of nonionized water, and then add them to the above primary emulsion. Stir at 450 rpm, and add water to bring the emulsion mass to 1000g. Shear the emulsion at 6000 rpm for 3 minutes, and homogenize it three times under high pressure at 45 MPa to obtain milk thistle seed oil emulsion, which is then sterilized and stored.

[0071] Example 7

[0072] Weigh 130g of nonionized water, add 24.0g of sucrose fatty acid ester, stir until evenly dispersed, heat to 75℃, and after the sucrose fatty acid ester has fully swollen into a paste, add 140g of propylene glycol and 80g of glycerol, dissolve, then add 12g of hexaglycerol monopalmitate, 3g of vitamin E polydiethanol succinate, and 3g of sorbitol, and stir evenly. This is the aqueous phase.

[0073] Weigh 550g of camellia seed oil, add 5g of mixed tocopherols, 2g of ascorbyl palmitate, 2g of rosemary extract, and 2.0g of polyglycerol ricinoleate, and dissolve by sonication at 55℃. This is the oil phase.

[0074] The oil phase is slowly added to the aqueous phase while maintaining the temperature at 60°C and a stirring speed of 500 rpm to form a primary emulsion.

[0075] Weigh out 3g of ascorbic acid and 6g of sodium ascorbate, dissolve them in 30g of non-ionized water, and then add them to the above primary emulsion. Stir at 500 rpm, and add water to bring the emulsion mass to 1000g. Shear the emulsion at 5000 rpm for 5 minutes, and homogenize it three times under high pressure at 40MPa to obtain camellia seed oil emulsion, which is then sterilized and stored.

[0076] In summary, the following parameters were selected in the above embodiments 1-7, as shown in Table 1:

[0077] Table 1

[0078]

[0079] Table 1 above shows the selection and configuration of multiple parameters. It's worth noting that although the weight unit in the table is "g," these parameters can be flexibly scaled up or down proportionally in practical applications to adapt to different production scales and needs. Therefore, introducing the concept of "parts by weight" will be more practical and versatile. "Parts by weight" is a relative unit that keeps the proportions of each ingredient in the formula constant, while the total weight can be adjusted according to actual needs. Therefore, when understanding and applying the parameters in the above embodiments, the weight unit "g" can be considered as "parts by weight" rather than a fixed number of grams, to achieve greater flexibility and practicality.

[0080] A variety of primary emulsifiers were used, such as sucrose fatty acid esters and polyoxyethylene (20) sorbitan monooleate. These emulsifiers showed good emulsification effects in the experiment, indicating that different types of primary emulsifiers have a certain influence on the emulsion properties.

[0081] The dosage of the primary emulsifier was optimized to varying degrees to achieve the best emulsification effect.

[0082] The compatibility between the primary emulsifier and the oil phase was investigated. The amount of primary emulsifier was adjusted according to the amount of oil phase added. The best emulsification effect was obtained when the amount of primary emulsifier was 2.0% to 6.0% of the weight of the oil.

[0083] Propylene glycol and glycerol were used together as co-emulsifiers to assist the emulsifiers in their function and improve the stability of the emulsion in the experiment.

[0084] Emulsifier selection: In Examples 1-7, a variety of primary emulsifiers were selected, such as sucrose fatty acid esters and polyoxyethylene (20) sorbitan monooleate. These emulsifiers exhibited excellent emulsifying effects in the experiments, fully demonstrating that different types of primary emulsifiers have a significant impact on emulsion performance.

[0085] Optimize the amount of primary emulsifier: Examples 1-7 optimized the amount of primary emulsifier by finely adjusting the amount of primary emulsifier to achieve the best emulsification effect.

[0086] Oil phase and emulsifier compatibility study: Examples 1-7 not only conducted an in-depth study on the compatibility between the main emulsifier and the oil phase, but also selected the most suitable ratio of oil phase and main emulsifier to obtain the best emulsification effect and ensure the overall performance of the emulsion.

[0087] Table 1 lists the usage schemes of various primary emulsifiers. The oil-phase emulsifier mainly consists of mono- and diglyceride fatty acid esters, polyglycerol ricinoleate, and sucrose fatty acid esters (monoester <30%), with proportions varying between 0.6 parts by weight and 4.0 parts by weight. The aqueous-phase emulsifier mainly contains sucrose fatty acid esters and different types and proportions of polyoxyethylene esters (such as polyoxyethylene (20) sorbitan monooleate and polyoxyethylene (20) sorbitan monolaurate), with a total amount between 8.5 parts by weight and 24.0 parts by weight. Specifically, it includes:

[0088] (1) There are several combinations of oil-phase emulsifier formulations. One is 1.0 parts by weight of mono- and diglyceride fatty acid esters, another is 1.5 parts by weight of polyglycerol ricinoleate, and yet another is 4.0 parts by weight of sucrose fatty acid ester (monoester <30%). In addition, there are mixed formulations of 0.6 parts by weight of mono- and diglyceride fatty acid esters and 0.4 parts by weight of polyglycerol ricinoleate, as well as combinations of 1.0 parts by weight of mono- and diglyceride fatty acid esters and 0.4 parts by weight of sucrose fatty acid ester (monoester <30%). Furthermore, there are formulations using 1.75 parts by weight of sucrose fatty acid ester (monoester <30%) alone, and 2.0 parts by weight of polyglycerol ricinoleate alone.

[0089] (2) The formulations of aqueous emulsifiers also exhibit diversity. These include combinations of 8.5 parts by weight of sucrose fatty acid ester and 1.5 parts by weight of polyoxyethylene (20) sorbitan monooleate, as well as 9.5 parts by weight of sucrose fatty acid ester used alone. Additionally, there are formulations using 20 parts by weight of sucrose fatty acid ester alone, and 9 parts by weight of polyoxyethylene (20) sorbitan monooleate alone. Furthermore, there are formulations combining 8 parts by weight of sucrose fatty acid ester and 3.2 parts by weight of polyoxyethylene (20) sorbitan monolaurate, and formulations using 17.45 parts by weight and 24.0 parts by weight of sucrose fatty acid ester alone. These different emulsifier formulations are suitable for different types of emulsion preparation, and the stability and performance of the emulsion can be optimized by adjusting the ratio and type of oil-phase and aqueous-phase emulsifiers.

[0090] Optimize the dosage of co-emulsifiers: Propylene glycol and glycerol were selected as co-emulsifiers and their ratio was optimized. The optimized combination of main emulsifiers can enhance the emulsification effect of the main emulsifiers and improve the stability of the emulsion.

[0091] The optimization of oxidant dosage was investigated. The aqueous phase antioxidants mainly consisted of ascorbic acid and sodium ascorbate, with different ratios of D-isoascorbate sodium. The oil phase antioxidants mainly included rosemary extract, mixed tocopherols, ascorbate palmitate, and synthetic tert-butylhydroquinone and butylated hydroxytoluene, with proportions varying between 1 and 5 parts by weight. Table 1 includes the following schemes:

[0092] (1) There are several combinations of aqueous antioxidant formulations. One is a mixture of 3 parts by weight of ascorbic acid and 8 parts by weight of sodium ascorbate; another is the use of 2 parts by weight of sodium ascorbate alone; yet another is a combination of 3 parts by weight of ascorbic acid and 15 parts by weight of sodium ascorbate, and 10 parts by weight of sodium ascorbate alone. In addition, there are 6 parts by weight of sodium D-isoascorbate alone, and a mixture of 3 parts by weight of ascorbic acid and 6 parts by weight of sodium D-isoascorbate or 6 parts by weight of sodium ascorbate.

[0093] (2) The formulations of oil-phase antioxidants are also diverse. These include combinations of 4 parts by weight of rosemary extract and 1 part by weight of mixed tocopherols, and combinations of 1.8 parts by weight of mixed tocopherols and 0.2 parts by weight of ascorbyl palmitate; there are also formulations using 2 parts by weight of mixed tocopherols alone and 2 parts by weight of rosemary extract alone. There are also synthetic antioxidant combinations of 2 parts by weight of tert-butylhydroquinone and 1 part by weight of butylated hydroxytoluene, and combinations of 5 parts by weight of mixed tocopherols, 2 parts by weight of ascorbyl palmitate, and 2 parts by weight of rosemary extract. These different antioxidant formulations are suitable for products with different needs and conditions to maintain their stability and prevent oxidation.

[0094] Example 8

[0095] The emulsion samples from Examples 1-7 were used as raw materials to prepare end-product flavored beverages, numbered Beverages 1-7. The formula was as follows: 32.3 parts oil emulsion, 6.67 parts xylitol, 1.67 parts fructooligosaccharides, 0.07 parts L-carnitine, 0.07 parts citric acid, 0.03 parts malic acid, 0.5 parts milk flavoring, 0.17 parts yogurt flavoring, 0.33 parts orange flavoring, and 58.19 parts deionized water. Each material was weighed according to the above formula, mixed thoroughly, and then sterilized and stored.

[0096] Evaluate the sensory state, centrifugal stability, and accelerated stability of the end product.

[0097] Comparative Example 1 (Comparing the effect of the type of primary emulsifier on salt tolerance, using an ionic emulsifier)

[0098] Based on Example 1, to compare the effect of the type of primary emulsifier on salt tolerance, ionic emulsifiers were used to prepare samples in this comparative example.

[0099] Weigh 340g of nonionized water, add 10g of citrate monoglyceride fatty acid ester, stir until evenly dispersed, heat to 75℃, and after fully swelling, add 50g of propylene glycol and 76g of glycerol, dissolve, then add 8g of octaglycerol monooleate, 1g of vitamin E polydiethanol succinate, and 1g of sorbitol, and stir evenly. This is the aqueous phase.

[0100] Weigh out 160g sunflower seed oil, 150g soybean oil, and 150g corn oil, add 4g rosemary extract and 1.0g mono- and diglyceride fatty acid esters, and dissolve by sonication at 60℃. This is the oil phase.

[0101] The remaining formulation and process are the same as in Example 1, and a vegetable oil emulsion is prepared.

[0102] Comparative Example 2 (comparing the effect of main emulsifier composition on emulsion centrifugal stability, without adding oil phase emulsifier)

[0103] Based on Example 1, the effect of the composition of the main emulsifier on the centrifugal stability of the emulsion was compared. In this comparative example, no oil phase emulsifier was added.

[0104] Weigh 340g of nonionized water, add 8.5g of sucrose fatty acid ester and 1.5g of polyoxyethylene (20) sorbitan monooleate, stir until evenly dispersed, heat to 75℃, and after fully swelling, add 50g of propylene glycol and 76g of glycerol, dissolve, then add 8g of polyoctaglycerol monooleate, 1g of vitamin E polydiethanol succinate and 1g of sorbitol, stir evenly, this is the aqueous phase.

[0105] Weigh out 160g sunflower seed oil, 150g soybean oil, and 150g corn oil, add 4g rosemary extract, and dissolve by sonication at 60℃. This is the oil phase.

[0106] The remaining formulation and process are the same as in Example 1, and a vegetable oil emulsion is prepared.

[0107] Comparative Example 3 (Comparing the effect of co-emulsifiers on the sterilization stability of emulsions, using only propylene glycol)

[0108] Based on Example 1, the effect of co-emulsifiers on the sterilization stability of emulsions was compared. In this comparative example, only propylene glycol was used as the co-emulsifier.

[0109] Weigh 340g of nonionized water, add 8.5g of sucrose fatty acid ester and 1.5g of polyoxyethylene (20) sorbitan monooleate, stir until evenly dispersed, heat to 75℃, and after fully swelling, add 50g of propylene glycol, dissolve, then add 8g of octaglycerol monooleate, 1g of vitamin E polydiethanol succinate and 1g of sorbitol, stir evenly, this is the aqueous phase.

[0110] Weigh out 160g sunflower seed oil, 150g soybean oil, and 150g corn oil, add 4g rosemary extract and 1.0g mono- and diglyceride fatty acid esters, and dissolve by sonication at 60℃. This is the oil phase.

[0111] The remaining formulation and process are the same as in Example 1, and a vegetable oil emulsion is prepared.

[0112] Comparative Example 4 (Comparing the effect of no stabilizer added on the pH stability of the emulsion)

[0113] Based on Example 1, the effect of not adding stabilizers on the pH stability of the emulsion was compared.

[0114] Weigh 340g of nonionized water, add 8.5g of sucrose fatty acid ester and 1.5g of polyoxyethylene (20) sorbitan monooleate, stir until evenly dispersed, heat to 75℃, and after fully swelling, add 50g of propylene glycol and 76g of glycerol, stir evenly, this is the aqueous phase.

[0115] Weigh out 160g sunflower seed oil, 150g soybean oil, and 150g corn oil, add 4g rosemary extract and 1.0g mono- and diglyceride fatty acid esters, and dissolve by sonication at 60℃. This is the oil phase.

[0116] The remaining formulation and process are the same as in Example 1, and a vegetable oil emulsion is prepared.

[0117] Comparative Example 5 (Effect of stabilizer composition on emulsion heat resistance and freeze-thaw resistance)

[0118] Based on Example 1, the effect of stabilizer composition on the heat resistance and freeze-thaw resistance of the emulsion was investigated. In this comparative example, only polyglycerol fatty acid esters were used as stabilizers.

[0119] Weigh 340g of nonionized water, add 8.5g of sucrose fatty acid ester and 1.5g of polyoxyethylene (20) sorbitan monooleate, stir until evenly dispersed, heat to 75℃, and after fully swelling, add 50g of propylene glycol and 76g of glycerol, dissolve, then add 8g of octaglycerol monooleate and stir evenly. This is the aqueous phase.

[0120] Weigh out 160g sunflower seed oil, 150g soybean oil, and 150g corn oil, add 4g rosemary extract and 1.0g mono- and diglyceride fatty acid esters, and dissolve by sonication at 60℃. This is the oil phase.

[0121] The remaining formulation and process are the same as in Example 1, and a vegetable oil emulsion is prepared.

[0122] Comparative Example 6 (Comparing the effect of antioxidants on the chemical stability of emulsions)

[0123] Based on Example 1, the effect of antioxidants on the chemical stability of the emulsion was investigated. In this comparative example, no oil phase antioxidants were added.

[0124] Weigh 340g of nonionized water, add 8.5g of sucrose fatty acid ester and 1.5g of polyoxyethylene (20) sorbitan monooleate, stir until evenly dispersed, heat to 75℃, and after fully swelling, add 50g of propylene glycol and 76g of glycerol, dissolve, then add 8g of polyoctaglycerol monooleate, 1g of vitamin E polydiethanol succinate and 1g of sorbitol, stir evenly, this is the aqueous phase.

[0125] Weigh out 160g sunflower seed oil, 150g soybean oil, and 150g corn oil, add 1.0g mono- and diglyceride fatty acid esters, and dissolve by sonication at 60℃. This is the oil phase.

[0126] The remaining formulation and process are the same as in Example 1, and a vegetable oil emulsion is prepared.

[0127] Effect Comparison Group 1. Emulsion State Evaluation

[0128] The emulsions prepared in Examples 1-7 and Comparative Examples 1-6 were evaluated, and the indicators included emulsion state, emulsion particle size, rehydration properties and centrifugal stability. The results are shown in Table 2.

[0129] Particle size determination method: The particle size of the emulsion was determined using a laser particle size analyzer. Particle size is one of the indicators for monitoring emulsion stability; larger particle sizes indicate poorer emulsion stability and a greater likelihood of emulsion breakage and oil separation.

[0130] Centrifugal stability test method: Place 10 mL of emulsion in a centrifuge tube, centrifuge at 4000 rpm for 10 min, and observe the state after centrifugation. Centrifugal stability can directly indicate the stability of the emulsion. Unstable emulsions will show water-emulsion separation, oil-emulsion separation, etc. after centrifugation.

[0131] The results show that the emulsions in Examples 1-7 have good stability, while the emulsion particle size in Comparative Examples 1-5 is increased and the volume of the emulsion layer is reduced after centrifugation. Comparative Examples 1 and 2 show slight oil floating phenomenon after reconstitution.

[0132] Table 2. Results of Emulsion State Evaluation

[0133]

[0134] The table showing the emulsion state evaluation results displays the test results for emulsion state, particle size, reconstitution properties, and centrifugal stability in different examples and comparative examples. Further analysis of these results follows:

[0135] Emulsion state and particle size: According to the results in the table, the emulsion state of the examples is "homogeneous," indicating that these emulsions have good stability. In contrast, in the comparative examples, the emulsion state of Comparative Example 1 is "slightly oily," and the particle sizes of Comparative Examples 1 and 2 are relatively large, indicating that these two groups of emulsions have poor stability. Furthermore, the emulsion particle sizes of the examples are small, concentrated between 0.58 and 0.79 μm, indicating that the small particle size of these emulsions is beneficial to improving emulsion stability.

[0136] Reconstitution properties: Data on reconstitution properties show that all examples exhibited good homogeneity and no oil drift at 20x, 50x, and 100x dilutions, indicating that these emulsions have good dispersibility and stability during reconstitution. Comparative Examples 1 and 2, however, showed poor performance, with small oil droplets appearing after reconstitution.

[0137] Centrifugal stability: The centrifugal stability data show that the emulsion volume of the examples is greater than 99.8%, exhibiting extremely high stability. In contrast, the emulsion volumes of Comparative Examples 1, 2, 4, and 5 are 98.0%, 95.0%, 96.5%, and 98%, respectively, which differs from the examples.

[0138] Comparative Examples 3 and 6 were no different from the Examples in terms of emulsion state, and other indicators such as accelerated stability and thermal stability need to be examined.

[0139] Effect Comparison Group 2. Accelerated Stability Assessment of Emulsion

[0140] Examples 1-4 and Comparative Examples 1-6 were subjected to accelerated testing at 57°C. The emulsion state was observed and the peroxide value (based on oil) was measured. The results are shown in Table 3.

[0141] In the examples, the emulsion remained uniform and stable in the later stages of acceleration, while in the comparative examples, the emulsion exhibited problems such as oil drift, separation, and increased peroxide value as the acceleration time increased.

[0142] Table 3 Results of accelerated stability study of emulsions

[0143]

[0144] Based on the table of accelerated stability test results for the emulsions, we can further analyze the performance of the emulsions during the acceleration process. The following is a comparative analysis of these data:

[0145] Emulsion state: The emulsions in the examples maintained a uniform and stable state at 5, 10, and 20 days of acceleration, without any oil drift or separation. However, the emulsions in the comparative examples showed varying degrees of problems in the later stages of acceleration. For example, Comparative Example 1 showed severe oil drift in the later stages of acceleration, while Comparative Examples 2-5 showed water-emulsion separation in the later stages of acceleration.

[0146] Peroxide value: The peroxide value of the emulsions in the examples showed a relatively stable trend during the acceleration process. The increase in peroxide value of the emulsion in Comparative Example 1 was due to the increased oxidation caused by oil leaching in the emulsion, while Comparative Example 6 also showed an increase in peroxide value because no antioxidant was added.

[0147] Effect Comparison Group 3. Evaluation of Emulsion Thermal Stability

[0148] The thermal stability of the emulsion includes low-temperature stability and high-temperature stability. Freeze-thaw tests and high-temperature sterilization tests were conducted on Examples 1-4 and Comparative Examples 1, 3, 4, and 5, respectively. The test results are shown in Table 4. The Examples showed excellent freeze-thaw stability and sterilization stability, and the particle size of the treated emulsions did not increase significantly, indicating excellent thermal stability. However, Comparative Examples 1, 3, 4, and 5 all showed demulsification and stratification after repeated freeze-thaw cycles and high-temperature sterilization.

[0149] Table 4 Results of emulsion thermal stability evaluation

[0150]

[0151] Based on the above table of emulsion thermal stability evaluation results, the stability performance of the emulsion under different temperature conditions can be further analyzed. The following is a comparative analysis of these data:

[0152] Freeze-thaw test: The emulsions in the examples maintained a homogeneous and stable state after 10 repeated freeze-thaw cycles, without any demulsification or stratification. In contrast, Comparative Examples 1, 3, 4, and 5 all exhibited varying degrees of demulsification and stratification after the freeze-thaw test, with Comparative Examples 1, 3, and 5 showing slight stratification and Comparative Example 4 showing severe stratification. Furthermore, the particle size variation in the examples was relatively small, indicating good low-temperature stability.

[0153] High-temperature sterilization test: The emulsions in the examples remained homogeneous and stable after high-temperature sterilization, with no significant increase in particle size. In contrast, Comparative Examples 1, 3, 4, and 5 all exhibited varying degrees of demulsification and stratification after high-temperature sterilization. Comparative Examples 1, 3, and 5 showed slight stratification, while Comparative Example 4 showed severe stratification. Furthermore, the comparative examples showed greater particle size variation, indicating poor high-temperature stability.

[0154] Effect Comparison Group 4. Performance Evaluation of Emulsion Application

[0155] The application performance of the emulsions in Examples 1-4 and Comparative Examples 1 and 4 was investigated.

[0156] The emulsion was added at a concentration of 10% to solutions of different pH values. The state of the emulsion was observed and accelerated testing was conducted. The results are shown in Table 5. The emulsion was added at a concentration of 10% to solutions of different ions. The state of the emulsion was observed and accelerated testing was conducted. The results are shown in Table 6.

[0157] As can be seen from the results in the table, Examples 1 to 4 can maintain a uniform and stable state in various application environments, while Comparative Examples 1 and 4 show problems such as flocculation, oil floating, and stratification.

[0158] Table 5 Results of application of emulsions under different pH conditions

[0159]

[0160] Table 6 Results of the application of emulsions under different ionic environments

[0161]

[0162] Based on the above table of emulsion application performance results, we can further analyze the performance of the emulsion under different application environments. The following is a comparative analysis of these data:

[0163] Different pH environments: The emulsions in the examples remained homogeneous and stable after being added to solutions of different pH values, without issues such as flocculation, oil leaching, or stratification. In contrast, Comparative Examples 1 and 4 exhibited varying degrees of oil leaching and stratification at pH 7 and pH 9, indicating that these emulsions had poor stability at higher pH environments.

[0164] Different ionic environments: The emulsions in the examples maintained a homogeneous and stable state after being added to solutions with different ionic compositions, without exhibiting problems such as flocculation or stratification. However, Comparative Example 1, when added to solutions containing Na... + K + Mg 2+ Ca 2+ All solutions exhibited varying degrees of stratification and oil leaching after being added to solutions containing Mg. Comparative Example 4, after being added to solutions containing Mg... 2+、 Ca 2+ The slight stratification observed after the solution was prepared indicates that these emulsions have poor stability under specific ionic conditions.

[0165] Effect Comparison Group 5. Performance Evaluation of Terminal Beverages

[0166] The performance of the final beverage in Example 8 was evaluated, including sensory evaluation, centrifugal stability, and accelerated stability.

[0167] Table 7 Results of the investigation of emulsions in finished beverages

[0168]

[0169] Based on the above test data, the final beverages in Example 8 exhibited good performance in terms of sensory evaluation, centrifugal stability, and accelerated stability. All beverages were assessed as homogeneous, flowable liquids with no stratification or oil floating. In the centrifugal stability test, all beverages remained stable without oil floating. In the accelerated stability test, all beverages remained homogeneous after 20 days of accelerated testing at 57°C, with no stratification or oil floating.

[0170] Based on the above analysis, the following conclusions can be drawn: the final beverage in Example 8 exhibits good stability in performance evaluation, whether in terms of sensory evaluation, centrifugal stability, or accelerated stability.

[0171] The above description is merely a preferred embodiment of the present invention, but the scope of protection of the present invention is not limited thereto. Any variations or substitutions that can be easily conceived by those skilled in the art within the scope of the technology disclosed in the present invention should be included within the scope of protection of the present invention. Therefore, the scope of protection of the present invention should be determined by the scope of the claims.

Claims

1. A high oil loading emulsion resistant to high temperature, acid, base and salt, characterized in that, The raw materials include the following components by weight parts: oil and fat 40-55 parts, main emulsifier 0.8-3.0 parts, stabilizer 0.8-2.0 parts, antioxidant 0.2-2.0 parts, co-emulsifier 10-35 parts, deionized water 12.5-40 parts; The main emulsifier includes oil phase emulsifier and water phase emulsifier; the oil phase emulsifier is selected from one or more of monoglyceride fatty acid ester, sucrose fatty acid ester with a monoglyceride content of less than 30%, and polyglycerol ricinoleate; the water phase emulsifier is selected from one or more of sucrose fatty acid ester and polyoxyethylene sorbitan fatty acid ester; the oil phase emulsifier accounts for 0.2-1.0% of the weight of the oil and fat, and the weight ratio of the water phase emulsifier to the oil phase emulsifier is (3-15):1; The weight ratio of the co-emulsifier to the deionized water is (0.8-5.5):3; the co-emulsifier is composed of propylene glycol and glycerol at a weight ratio of 1:(0.5-5); The stabilizer is a combination of polyglycerol fatty acid ester, vitamin E polyethylene glycol succinate and sorbitol, the glycerol polymerization degree of the polyglycerol fatty acid ester is 6-10, and the polyglycerol fatty acid ester accounts for more than 50wt% in the stabilizer; The antioxidant includes water phase antioxidant and oil phase antioxidant; the water phase antioxidant is selected from one or more of ascorbic acid, sodium ascorbate and D-sodium erythorbate; the oil phase antioxidant is selected from one or more of mixed tocopherols, ascorbyl palmitate, rosemary extract, tert-butyl hydroquinone and butylated hydroxytoluene.

2. The high oil load emulsion of claim 1, wherein, The oil and fat is selected from one or more of sunflower oil, rapeseed oil, soybean oil, corn oil, flaxseed oil, safflower oil, coconut oil, oil tea seed oil, milk thistle seed oil, olive oil, palm oil, cottonseed oil, peanut oil, perilla seed oil, evening primrose oil, grape seed oil, almond oil, walnut oil, castor oil, rice bran oil, tiger nut oil, blueberry seed oil, babassu oil, sugar maple seed oil, avocado oil, fish oil, DHA algal oil, medium-chain triglyceride, conjugated linoleic acid glyceride, and diglyceride oil.

3. The method for preparing the high-temperature resistant, acid and alkali resistant, and salt resistant high-oil-carrying emulsion according to claim 1, characterized in that, The method comprises the following steps: S1. Weigh the deionized water, add the water phase emulsifier, and make it uniformly dispersed and then heated and dissolved, add the co-emulsifier after complete dissolution, and stir until the main emulsifier and the co-emulsifier are fully dissolved and the state is uniform; add the stabilizer and stir until complete dissolution, at this time the water phase is transparent to translucent; S2. Weigh the oil and fat according to the formula, add the oil phase emulsifier and the oil phase antioxidant, and fully dissolve to obtain the oil phase; S3. Under continuous stirring, slowly add the oil phase to the water phase, fully stir to form the initial emulsion; S4. Add the water phase antioxidant to the initial emulsion, continue to stir until the system is uniform, and then perform high-speed shearing and high-pressure homogenization to prepare the emulsion.

4. The method of claim 3, wherein, The water phase emulsifier in S1 is dissolved at a temperature of 70-75℃; the oil phase emulsifier and the oil phase antioxidant in S2 are dissolved at a temperature of 50-60℃.

5. The method of claim 3, wherein, The emulsification temperature in S3 is 50-60℃.

6. The application of the high-temperature-resistant, acid-and-alkali-resistant and salt-resistant high oil-loading emulsion of claim 1 in the field of liquid beverages.

7. The use of the high temperature, acid, base and salt resistant high internal phase emulsion with high oil loading according to claim 1 in the field of oral liquids.

8. The use of the high temperature, acid, base and salt resistant high internal phase emulsion with high oil loading according to claim 1 in the field of dietary supplements.

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