Formula of a low or isotonic antifreeze-thaw emulsion, emulsion, preparation method and application thereof
Through the combination of specific raw and auxiliary materials and preparation processes, the problem of poor freeze-thawing stability of the emulsion under low or isoosmotic pressure is solved, and emulsions with high oil-carrying and good oxidation stability are prepared, which are suitable for a variety of food fields and reduce transportation and storage costs.
Patent Information
- Application Number
- CN202310596193.0
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2023-05-25
- Publication Date
- 2025-08-12
- Estimated Expiration
- 2043-05-25
AI Technical Summary
The existing emulsions have poor stability during freezing and thawing, prone to demulsification and stratification, and commonly used chemical synthetic antifreeze agents have safety risks. The existing technology has failed to effectively solve the problem of antifreeze-thaw stability under low or isoosmotic pressures.
Using specific combinations of raw and auxiliary materials and addition sequences, low or isoosmotic oil emulsions with low or isoosmotic pressure are prepared through multiple shearing and high pressure homogenization, including vegetable oil, denatured starch, diglycerides, dietary fiber and antioxidants, and the osmotic pressure is controlled at 100-320mOsm/kgH2O to ensure that the emulsion remains stable during freeze-thawing.
Prepare emulsions with high oil-carrying oil, good oxidation stability and anti-freeze-thaw stability, adapt to temperature changes, reduce transportation and storage costs, and avoid safety hazards of chemical synthesis of antifreezes. They are suitable for a variety of food fields.
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Abstract
Description
Technical Field
[0001] The present invention belongs to the technical field of emulsions, and in particular relates to a formula of a low or isotonic antifreeze-thaw emulsion, the emulsion, a preparation method and application thereof. Background Art
[0002] As we all know, osmotic pressure is a necessary condition for osmotic action in the human body and is an important indicator involved in biochemistry. The osmotic pressure of human plasma is about 300mOsm / kgH2O, while the osmotic pressure of breast milk is slightly lower. This indicator is closely related to the human metabolic system and health. The Codex Alimentarius Commission, the European Union, and the Australian and New Zealand Food Standards all stipulate that osmotic pressure must be marked on the labels of special medical purpose formula foods. As more and more functional foods enter the public's field of vision, this indicator deserves extra attention from the perspectives of nutrition, safety, and market supervision. However, at present, there are relatively few studies on osmotic pressure in functional foods by scholars at home and abroad, and my country has not yet completed the formulation of relevant standards for osmotic pressure in functional foods.
[0003] Functional foods currently available on the market have complex matrices and diverse sample forms, including liquid, semi-solid, and solid forms, such as powders, emulsions, and fat emulsions. Due to their varying functional effects, their osmotic pressures vary, and the requirements for osmotic pressure measurements for foods in different sample forms vary. Emulsion technology is widely used in the food industry, serving as an effective means of improving the nutritional properties of foods by reducing fat content and / or incorporating water-soluble nutrients and flavorings. However, emulsion products may encounter temperature fluctuations during transportation, storage, and use, leading to stability issues. Common oil / water emulsions in the prior art all experience structural damage upon freezing, with coagulation or oil-water separation occurring, making them intolerant to freezing or repeated thawing. This is because the emulsion is partially water, which freezes when exposed to low temperatures. The formation of ice crystals during freezing reduces the space between droplets, potentially causing interfacial membrane rupture and promoting the aggregation of water droplets. Therefore, both freezing and thawing affect the stability of the emulsion. Consequently, most commercial emulsions specify specific storage temperature requirements. In my country, the temperature in most winters is below 0°C, and in some areas it is even below -20°C. If the global supply chain is taken into account, the temperature difference will be even greater, which places higher requirements on the stability of the emulsion during transportation and storage. Otherwise, a lot of costs will be invested in the temperature control supply chain process.
[0004] Studies have shown that maintaining an emulsion at a higher osmotic pressure improves its freeze-thaw resistance. During the freeze-thaw process, higher osmotic pressures allow for partial water release from the emulsion microspheres, reducing the impact of ice crystals generated during freezing. However, lower osmotic pressures lead to excessive interstitial water content. As ice crystals accumulate during freezing, they rupture the interfacial membrane, potentially causing irreversible damage and leading to demulsification and delamination during thawing. Therefore, lower osmotic pressures make it more difficult to improve the freeze-thaw stability of emulsions. Common freeze-thaw-resistant products often require the addition of chemically synthesized antifreeze agents, such as propylene glycol and polyethylene glycol, which pose safety risks. Alternatively, they require the addition of large amounts of aqueous stabilizers and buffer salts, which inevitably increase the product's osmotic pressure. In this context, optimizing preparation techniques or adding natural substances to achieve emulsion products with lower or isotonic pressures, high encapsulation efficiency, and excellent oxidative stability and freeze-thaw stability remains a pressing challenge.
[0005] The prior art documents a series of research results on related freeze-thaw-resistant emulsion preparations or foods with low or equal osmotic pressures: CN104940939B discloses a technical solution: an aqueous phase containing glycerol (preferably 7.5%-15.0%) and water is dissolved in a specific ratio, an oil phase is added, the pH of the system is adjusted to between 4.5 and 10.1 after stirring, and finally homogenized five times using a microfluidizer at a pressure of 14,000 psi to obtain a fat emulsion with excellent freeze-thaw resistance. CN104770559A discloses a technical solution: soy protein isolate is modified with papain, the raw oil and the modified protein product are mixed with distilled water to form a solution with a protein concentration of 2%, the pH is adjusted to 7.0, 20% soybean oil is added, and the emulsion is prepared using a high-speed homogenizer at 20,000 rpm for 2 minutes, thereby improving the original freeze-thaw resistance. Similarly, CN113397122A discloses a technical solution that involves desalting salted egg white gel, mixing it with water, and centrifuging to obtain a desalted salted egg white nanogel particle solution. This solution is then mixed with a sodium alginate solution, and then an oil phase is added and stirred to obtain a base emulsion. A calcium carbonate dispersion and a gluconolactone solution are then added, respectively, and finally stirred in a high-speed disperser at 10,000 rpm to obtain a Pickering emulsion, thereby improving the original freeze-thaw resistance. CN111280290 discloses a technical solution that involves heating milk to 65°C, then adding monoglyceride and diglyceride fatty acids, sodium caseinate, phospholipids, dipotassium hydrogen phosphate, sodium carboxymethyl cellulose, and white sugar, stirring to dissolve, and then adding yogurt to obtain a colloidal solution, which is then evenly mixed and frozen to obtain the corresponding ice cream, which has a good taste and flavor after freeze-thaw. CN101356988A discloses a technical solution in which whey protein isolate is dissolved in a calcium carbonate solution, sugar solution is added, the mixture is mixed, citric acid is used to adjust the pH, nutrients and flavoring substances are added, and purified water is added to obtain a corresponding emulsion beverage having an osmotic pressure of 303 mOsm / kgH2O per liter. CN108056353A discloses a technical solution in which corn starch, cyclodextrin, sucrose, glucose, sodium chloride, a chitosan derivative, and all organic acids are mixed, flavorings are added, and the mixture is mixed with purified water, followed by granulation and drying to obtain acidic granules. The remaining material is mixed with sodium bicarbonate to obtain alkaline granules. Finally, the two granules are uniformly mixed to obtain an isotonic solid beverage containing a chitosan derivative. The solution obtained by dissolving the mixture in water has an osmotic pressure of 280-320 mOsm / kgH2O. These patents disclose methods for preparing freeze-thaw-resistant emulsion formulations or foods with low or isotonic pressure, but no technical means are disclosed that address both requirements. The general preparation methods of antifreeze-thaw emulsions mostly involve modifying the raw wall materials, or adding more pH regulators, stabilizers and antifreeze agents to the preparations, which undoubtedly brings hidden dangers to the safety and health of the products.However, there are relatively few patents that focus on the osmotic pressure of food, and they do not consider the freeze-thaw stability problems caused by lower or equal osmotic pressure, which will bring a series of problems to the actual production, sales and transportation of the product. Summary of the Invention
[0006] To address the problems described in the prior art, the present invention provides a formula for a low or isotonic antifreeze-thaw emulsion, an emulsion, a preparation method, and applications thereof. Taking into account subsequent production and practical application issues, the present invention selects a specific combination of raw and auxiliary materials and a different order of addition to produce a fat emulsion with low or isotonic pressure, high oil loading, and excellent oxidative stability and antifreeze-thaw stability.
[0007] First, the formula of the low or isotonic antifreeze-thaw emulsion described in the first aspect of the present invention comprises the following components in parts by weight:
[0008]
[0009] For the above-mentioned formula technical solution, preferably, the oil includes one or more of various vegetable oils (such as soybean oil, sunflower oil, linseed oil, conjugated linoleic acid glyceride, medium-chain triglycerides, pumpkin seed oil, tomato seed oil, docosahexaenoic acid oil, eicosapentaenoic acid oil, etc.) and animal fats (such as butter, fish oil, etc.); the amount of oil added is preferably 21-38 parts by weight, and the optimal range is 30-34 parts by weight.
[0010] In the above-mentioned formula technical solution, preferably, the modified starch mainly refers to sodium starch octenylsuccinate; the added amount of the modified starch is preferably 6-13 parts by weight, and the optimal range is 8-11 parts by weight.
[0011] In the above-mentioned formulation technical solution, preferably, the diglyceride is selected from one or a mixture of olive seed oil diglyceride oil, soybean oil diglyceride oil, linseed oil diglyceride oil, rapeseed oil diglyceride, safflower oil diglyceride, sunflower oil diglyceride and corn oil diglyceride oil.
[0012] In the above-mentioned technical solution, preferably, the purity of the diglyceride is 10-90 wt %. Considering the freeze-thaw resistance, the purity is preferably 40-60 wt %.
[0013] In the technical solution of the preparation method described above, preferably, the diglyceride is used in an amount of 5.0-12.5 parts by weight; considering the freeze-thaw resistance, the amount is 7.5-10 parts by weight;
[0014] In the above-mentioned formula technical solution, preferably, the dietary fiber includes one or a mixture of several of resistant dextrin, inulin, isomaltooligosaccharide, fructooligosaccharide, lacto-oligosaccharide, xylo-oligosaccharide, soybean oligosaccharide and polydextrose.
[0015] In the above-mentioned formula technical solution, preferably, the dietary fiber is added in an amount of 6-13 parts by weight, and the optimal range is 8-10 parts by weight. Considering the anti-freeze-thaw properties, the dietary fiber is preferably added in an amount of 5-15 parts by weight.
[0016] In the above-mentioned formula technical solution, preferably, the small molecule sugar includes at least one of sucrose, glucose syrup, white sugar, glucose powder, lactose or maltose.
[0017] In the above-mentioned formula technical solution, preferably, the amount of small molecule sugar added is 2-7 parts by weight, and the optimal range is 3-5 parts by weight.
[0018] In the above-mentioned formulation technical solution, preferably, the antioxidant includes a water-phase antioxidant and an oil-phase antioxidant;
[0019] In the above-mentioned technical solution, preferably, the aqueous antioxidant is selected from one or a mixture of sodium ascorbate, ascorbic acid, sodium citrate and ascorbyl palmitate; further, the aqueous antioxidant is preferably sodium ascorbate and ascorbic acid; and the weight ratio of sodium ascorbate to ascorbic acid is in the range of (1-5): (1), more preferably (1-2): (1);
[0020] In the above-mentioned formulation technical solution, preferably, the oil-phase antioxidant is selected from one or a mixture of d-α-tocopherol, dl-α-tocopherol, mixed tocopherols, rosemary extract, phospholipids, butylated hydroxyanisole, antioxidant 264, and tert-butylhydroquinone. Among them, the oil-phase antioxidant is preferably mixed tocopherols, rosemary extract, phospholipids, or butylated hydroxyanisole.
[0021] For the above-mentioned formulation technical solution, preferably, the amount of the aqueous phase antioxidant used is 0.2-1.8 parts by weight;
[0022] In the above-mentioned technical solution, preferably, the amount of the oil-phase antioxidant used is 0.01-1.0 parts by weight;
[0023] Another aspect of the present invention is to protect a method for preparing a low or isotonic antifreeze-thaw emulsion using the above-mentioned formula, comprising the following steps:
[0024] (1) At 50-70°C, 5-15 parts by weight of modified starch are dispersed in 80-120 parts by weight of water, and after dissolution, 5-20 parts by weight of dietary fiber and 1-8 parts by weight of small molecule sugar are added and dissolved to adjust the osmotic pressure of the system to 100-250mOsm / kgH2O, more preferably 150-230mOsm / kgH2O, and the optimal osmotic pressure is 180-220mOsm / kgH2O; then 0-2 parts by weight of aqueous antioxidant are added and dissolved to adjust the osmotic pressure of the system to 100-320mOsm / kgH2O, more preferably 220-310mOsm / kgH2O, and the optimal osmotic pressure is 260-290mOsm / kgH2O.
[0025] (2) adding 0.5-4 parts by weight of diglyceride and 0-2 parts by weight of oil-phase antioxidant to 20-40 parts by weight of oil, heating and stirring at 50-70° C.;
[0026] (3) mixing the liquids prepared in steps (1) and (2), emulsifying at 50-70° C., and then homogenizing at 50-70 MPa to complete the primary emulsification;
[0027] (4) Add 2.5-15 parts by weight of diglyceride to the liquid obtained in step (3), emulsify at 50-70° C., shear at 5000-8000 r / min for 2-5 min, homogenize at 20-40 MPa, perform secondary emulsification, and sterilize to obtain the final product.
[0028] In the technical solution of the preparation method described above, preferably, the amount of the diglyceride used in step (2) is 1.0-2.5 parts by weight, and considering the freeze-thaw resistance, it is further preferably 1.5-2 parts by weight;
[0029] In the technical solution of the preparation method described above, preferably, the amount of the diglyceride used in step (4) is 4.0-10 parts by weight; considering the freeze-thaw resistance, it is further preferably 6-8 parts by weight;
[0030] Another aspect of the present invention is to protect a low- or isotonic-pressure freeze-thaw-resistant emulsion prepared using the method described above. The emulsion has an osmotic pressure range of 100-320 mOsm / kgH2O, more preferably 250-320 mOsm / kgH2O. The emulsion remains homogeneous and stable after 5, 10, or even 20 freeze-thaw cycles, exhibits no demulsification or demixing, and retains the inherent flavor of the product.
[0031] Another aspect of the present invention is to protect the use of the low or isotonic antifreeze-thaw emulsion described above in the food field, including use in the preparation of beverages, energy drinks, functional drinks, liquid foods, juices, prepared dairy products, yogurt, cheese, ice cream, frozen desserts, complementary foods, seasonings, sauces and other food fields.
[0032] Beneficial effects of the present invention:
[0033] The present invention obtains a plant-based oil emulsion with low or isotonic pressure, high oil content, good oxidation stability and freeze-thaw stability through multiple shearing and high-pressure homogenization. The present invention selects a specific combination of raw and auxiliary materials, different addition orders and emulsification processes, breaks through the technical bottleneck of poor freeze-thaw stability at low or isotonic pressure, solves the difficulty of strict temperature control of the emulsion during transportation and storage, can effectively reduce its industrialization cost and improve quality, and the final emulsion is uniform in state, good in appearance, and has a high oil content, good oxidation stability, good product adaptability, acid and alkali resistance, avoids the acid resistance of protein system emulsions, and can be widely used in functional drinks, prepared dairy products, various sauces, ice cream and other food fields. The materials for preparing the emulsion are simple and easy to obtain, the process takes less time, is highly efficient, and is simple to operate. It avoids pollution such as organic reagents, is environmentally friendly, and has low cost. DETAILED DESCRIPTION
[0034] The following non-limiting examples are used to further illustrate the technical solutions and effects of the present invention and should not be construed as limiting the invention in any form. Unless otherwise specified, percentages in this specification are all weight percentages.
[0035] Example 1
[0036] Weigh 1000g of water into a 2000mL beaker at 60°C. Add 95g of modified starch and stir until completely dissolved. Then add 90g of resistant dextrin and 30g of glucose syrup, adjusting the osmotic pressure of the aqueous phase to 215mOsm / kg H2O. Add 9.5g of sodium ascorbate and 5.2g of ascorbic acid to the aqueous phase and stir until completely dissolved. The osmotic pressure of the entire system is measured to be 285mOsm / kg H2O. This is the aqueous phase. Then, weigh 330g of sunflower oil, 16g of 50% pure soybean diglyceride oil, and 0.3g of mixed tocopherols into a 1000mL beaker and mix thoroughly in a 60°C waterbath. This is the oil phase. After the oil phase is added to the aqueous phase, emulsify at 60°C and then homogenize twice at 60MPa. The remaining 64 g of 50% pure soybean diglyceride was added and emulsified at 60°C. The mixture was then sheared using a high-speed shearing machine at 6000 rpm for 4 minutes. Finally, the mixture was homogenized twice at 30 MPa to obtain the corresponding emulsion. The prepared emulsion was sterilized at high temperature and aseptically filled into aluminum bottles, designated as Sample 1.
[0037] Example 2
[0038] Weigh 1200g of water into a 2000mL beaker at 50°C. Add 65g of modified starch and stir until completely dissolved. Then add 65g of isomaltooligosaccharide and 22g of white sugar, adjusting the osmotic pressure of the aqueous phase to 185mOsm / kg H2O. Add 5.5g of sodium ascorbate and 4.3g of ascorbic acid to the aqueous phase and stir until completely dissolved. The osmotic pressure of the entire system is measured to be 222mOsm / kg H2O. This is the aqueous phase. Then, weigh 215g of docosahexaenoic acid (DHA) oil, 10g of 40% pure olive oil diglyceride, and 0.2g of rosemary extract into a 1000mL beaker and mix thoroughly in a 50°C waterbath. This is the oil phase. After the oil phase is added to the aqueous phase, emulsify at 50°C and then homogenize twice at 50MPa. The remaining 40 g of 40% pure olive oil diglyceride was added and emulsified at 50°C. The mixture was then sheared using a high-speed shearing machine at 5000 rpm for 3 minutes. Finally, the mixture was homogenized twice at 20 MPa to obtain an emulsion. The prepared emulsion was sterilized at high temperature and aseptically filled into an aluminum container, designated Sample 2.
[0039] Example 3
[0040] Weigh 800g of water into a 2000mL beaker at 70°C. Add 120g of modified starch and stir until completely dissolved. Then add 100g of oligofructose and 45g of sucrose, adjusting the osmotic pressure of the aqueous phase to 245mOsm / kg H2O. Add 10.0g of sodium ascorbate and 8.0g of ascorbic acid to the aqueous phase and stir until completely dissolved. The osmotic pressure of the entire system is measured to be 298mOsm / kg H2O. This is the aqueous phase. Then, weigh 380g of soybean oil, 22g of 60% pure linseed oil diglyceride, and 1.0g of d-α-tocopherol into a 1000mL beaker and mix thoroughly in a 60°C waterbath. This is the oil phase. After the oil phase is added to the aqueous phase, emulsify at 70°C and then homogenize twice at 60MPa. The remaining 88 g of 60% pure linseed oil diglyceride was added and emulsified at 70°C. The mixture was then sheared using a high-speed shearing machine at 8000 rpm for 5 minutes and homogenized twice at 30 MPa to obtain the corresponding emulsion. The prepared emulsion was sterilized at high temperature and aseptically filled into aluminum containers, designated Sample 3.
[0041] Example 4
[0042] The product performance of samples 1, 2, and 3 was evaluated, among which the centrifugation method was used to determine the stability of the emulsion. After high-speed centrifugation, the emulsion may show a certain degree of stratification and precipitation. The proportion of the precipitated layer mass to the total emulsion mass was measured. The smaller the proportion, the better the stability. It is generally believed that if the precipitation layer of the emulsion is accelerated for three months and is ≤3%, the product is qualified. This is an effective method for quickly judging the stability of the emulsion. The osmotic pressure detection method refers to "BJS 202102 Special Food Osmotic Pressure Determination", and the particle size is determined by "Laser Particle Size Analyzer". The final results are shown in Table 1:
[0043] Table 1
[0044]
[0045] The results show that the low or isotonic antifreeze-thaw emulsion obtained by the process disclosed in this application has a good appearance and smell, a small particle size, can be quickly dissolved upon dilution, has a uniform state, and an osmotic pressure lower than or equal to the human osmotic pressure (300mOsm / kgH2O), which is more beneficial to health and human absorption. In addition, centrifugal stability shows that it can have good storage stability. These properties all indicate that the product has excellent characteristics and can be used in the preparation of beverages, energy drinks, functional drinks, liquid foods, juices, prepared dairy products, yogurt, cheese, ice cream, frozen desserts, complementary foods, seasonings, sauces and other food fields.
[0046] Example 5
[0047] Samples 1, 2, and 3 were placed in an accelerated oven at 40°C and 75% humidity for three months to evaluate product stability. The results are shown in Table 2:
[0048] Table 2
[0049]
[0050]
[0051] From the accelerated stability experiment, it can be seen that after accelerating for 3 months, the outward appearance, the smell, the osmotic pressure of the three samples did not change significantly, and the peroxide value and the acid number increased slightly, but it is generally believed that the peroxide value accelerated for three months is less than or equal to 10.0meq / kg, and the acid number is less than or equal to 1.0mgKOH / g product is qualified. Wherein from the dilution effect in water and the emulsion appearance oily situation, although sporadic oil flowers appeared in the accelerated for 3 months, the emulsion flocculation, the oil phase polymerization and the stratification phenomenon that the obvious emulsion occurs easily did not occur, and the overall presentation was uniform and stable, and although the emulsion particle size increased slightly in the accelerated for three months, the overall presentation was normally distributed, which also proves that the emulsion stability is relatively good, and its centrifugal stability is identical with the particle size growth situation, and it is generally believed that the emulsion accelerated for three months has a separation layer less than or equal to 3%, and the product is qualified. The product prepared by the process of the application has excellent antioxidant stability and storage stability.
[0052] Example 6
[0053] The aluminum bottles filled with samples were sealed and placed in a -20°C refrigerator for 24 hours, and then placed at 25°C (room temperature) for 5 hours until completely thawed. This is considered one freeze-thaw cycle. The results after 1 to 20 freeze-thaw cycles are shown in Table 3:
[0054] Table 3
[0055]
[0056]
[0057] Freeze-thaw stability tests show that after two freeze-thaw cycles, although some oil flotation occurred after the emulsion dissolved, the overall consistency was uniform, with no signs of emulsion instability. The particle size increased slightly, but remained normally distributed. The requirement for a precipitation layer of ≤3% after five freeze-thaw cycles demonstrates excellent freeze-thaw stability. Samples 1 and 3 exhibited superior freeze-thaw resistance, which is attributed to the slightly lower water content and relatively higher osmotic pressure of the emulsions. Generally, the water content and osmotic pressure of an emulsion are inversely proportional to its freeze-thaw stability.
[0058] Example 7
[0059] Based on the process of Example 1, only the different purities of the diglyceride oil were replaced, and the effect of purity on the performance of the emulsion product was studied. The product status is shown in Table 4:
[0060] Table 4
[0061]
[0062] The measurement results after 5 freeze-thaw cycles are shown in Table 5:
[0063] Table 5
[0064]
[0065] The results show that while a diglyceride oil purity between 10% and 80% can achieve a homogeneous emulsion with sporadic or no oil flotation, after five freeze-thaw cycles, when the purity is below 40% or above 60%, the emulsion exhibits noticeable oil flotation or direct stratification, an increased oily odor, and even oily grease flotation after dilution. After centrifugation, the precipitated layer is greater than 3%, making the product unacceptable. However, when the diglyceride oil purity is between 40% and 60%, the particle size of the emulsion product only increases slightly, but maintains a normal distribution. Neither the appearance nor the solubility change. The percentage of the precipitated layer increases slightly, and products with a precipitated layer of ≤3% are generally considered acceptable. Therefore, it is essential to control the diglyceride oil purity within the range of 40% to 60% to achieve the desired freeze-thaw resistance.
[0066] Example 8
[0067] Based on the process of Example 1, the formula dosage and process parameters were not changed. Only the addition order of the diglyceride oil was adjusted. While the first diglyceride oil addition process remained unchanged, the effect of the second diglyceride oil addition process on the product performance was investigated. The product performance is shown in Table 6:
[0068] Table 6
[0069]
[0070]
[0071] The measurement results after 5 freeze-thaw cycles are shown in Table 7:
[0072] Table 7
[0073]
[0074] Judging from the results, the addition process sequence of the second diglyceride oil must be after high-pressure homogenization and high-speed shearing after addition, so as to obtain an emulsion with good odor, small particle size, rapid dissolution after dilution, uniform state, and no floating oil, as well as achieve good anti-freeze-thaw effect.
[0075] Example 9
[0076] Based on the process of Example 1, the formulation dosage and process parameters were not changed. Only the ratio of diglyceride oil added twice was changed. The effect of the oil addition ratio on product performance was investigated. The measurement results before and after one freeze-thaw cycle are shown in Table 8:
[0077] Table 8
[0078]
[0079]
[0080] The measurement results after 5 freeze-thaw cycles are shown in Table 9:
[0081] Table 9
[0082]
[0083] Judging from the results, diglyceride oil must be added in two times, and the ratio of the two additions must be 1:4 (the first addition amount must be controlled at 20%, and the second addition amount is the remaining 80%) to obtain an emulsion with good odor, small particle size, rapid dissolution upon dilution, uniform state, and no floating oil, as well as good anti-freeze-thaw effect.
[0084] Example 10
[0085] Based on the process of Example 1, the original formula materials and proportions were not changed, and only the emulsification step was adjusted. The effect of emulsification in batches on product performance was investigated. The state of the emulsion product is shown in Table 10:
[0086] Table 10
[0087]
[0088]
[0089] The measurement results after 5 freeze-thaw cycles are shown in Table 11:
[0090] Table 11
[0091]
[0092] Judging from the results, emulsification must be carried out twice to obtain an emulsion with good odor, small particle size, rapid dissolution upon dilution, uniform state, and no floating oil, as well as to achieve good freeze-thaw resistance.
[0093] Example 11
[0094] Based on Example 1, the original formula materials and process parameters were not changed. Only the amount of diglyceride was replaced. The effect of the amount of diglyceride on product performance and freeze-thaw stability was investigated. The product status is shown in Table 12. The test results after freeze-thaw cycles are shown in Table 12:
[0095] Table 12
[0096]
[0097]
[0098] The measurement results after 5 freeze-thaw cycles are shown in Table 13:
[0099] Table 13
[0100]
[0101] The results show that although a uniform emulsion can be achieved with a low amount of oil floating when the diglyceride dosage is between 3 and 19 parts, after one freeze-thaw cycle, if the diglyceride dosage is less than 5 parts or greater than 15 parts, the emulsion will exhibit noticeable oil floating, an increased oily odor, and even stratification after dissolution and dilution. After centrifugation, the precipitated layer is greater than 3%, making the product unqualified. However, when 5 to 15 parts of diglyceride are added, the particle size of the emulsion product only increases slightly, but shows a normal distribution, and the appearance and solubility remain unchanged. The percentage of the precipitated layer obtained by centrifugation increases slightly, and products with ≤3% after 5 freeze-thaw cycles are generally considered qualified. Therefore, the diglyceride dosage must be controlled within the range of 5 to 15 parts to achieve the corresponding freeze-thaw resistance effect; other ranges do not have this effect.
[0102] Example 12
[0103] Based on Example 1, the original formula ratio and process parameters were not changed. Only the diglyceride was replaced with other antifreeze-thaw agents or emulsifiers. The effect of other agents or emulsifiers that may have antifreeze-thaw effects on product performance was investigated. The emulsion state is shown in Table 14:
[0104] Table 14
[0105]
[0106] The measurement results after 5 freeze-thaw cycles are shown in Table 15:
[0107] Table 15
[0108]
[0109] Judging from the results, the effects of several other reagents or emulsifiers that may have anti-freeze-thaw effects were poor. The prepared emulsions were unqualified after 5 freeze-thaw cycles, and the precipitation layer was >3%. Although propylene glycol performed slightly better, it is a chemically synthesized reagent with questionable safety. The diglyceride oil used is not only of natural plant origin, but also has excellent effects. It can obtain an emulsion with good odor, small particle size, rapid dissolution upon dilution, uniform state, and no floating oil at a lower osmotic pressure, as well as achieve good anti-freeze-thaw effects. Other combinations of substances do not have this effect.
[0110] Example 13
[0111] Based on the process of Example 1, the original formula materials and process parameters were not changed. Only the amount of resistant dextrin and glucose syrup was changed. The osmotic pressure was controlled within different ranges. The effect of different osmotic pressures on product performance was investigated. The emulsion state is shown in Table 16:
[0112] Table 16
[0113]
[0114]
[0115] The results after 5 freeze-thaw cycles are shown in Table 17.
[0116] Table 17
[0117]
[0118]
[0119] The results show that different osmotic pressures are inversely proportional to the freeze-thaw resistance. The greater the osmotic pressure, the better the emulsion state and freeze-thaw stability. However, blindly increasing their proportions will undoubtedly increase the product osmotic pressure, thereby posing health risks. Therefore, by controlling the dietary fiber content to 5-15 parts and the small molecule sugar content to 1-8 parts, the emulsion osmotic pressure is ultimately controlled between 100-320mOsm / kgH2O (preferably 275mOsm / kgH2O). This is the optimal balance between low or isotonic pressure beneficial to health and emulsion quality, resulting in an emulsion with good freeze-thaw resistance. An emulsion osmotic pressure of 100-320mOsm / kgH2O is within the scope of protection of this invention.
[0120] 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 changes or substitutions that can be easily conceived by those skilled in the art within the technical scope disclosed in the present invention should be included in the scope of protection of the present invention. Therefore, the scope of protection of the present invention should be based on the scope of protection of the claims.
Claims
1. A low or isotonic antifreeze-thaw emulsion comprising the following components: 20-40 parts by weight of oil; 5-15 parts by weight of modified starch; 5-12.5 parts by weight of diglyceride with a purity of 40-60 wt%; 7-13 parts by weight of dietary fiber; 2-7 parts by weight of small molecule sugar; 0-4 parts by weight of antioxidant; 80-120 parts by weight of water; The preparation method thereof comprises the following steps: (1) Disperse 5-15 parts by weight of modified starch in 80-120 parts by weight of water at 50-70°C, add 7-13 parts by weight of dietary fiber and 2-7 parts by weight of small molecule sugar, dissolve them, and adjust the osmotic pressure of the system to 100-250mOsm / kgH2O; then add 0-2 parts by weight of aqueous antioxidant, dissolve them, and adjust the osmotic pressure of the system to 100-320mOsm / kgH2O; (2) Add 20% by weight of diglyceride and 0-2 parts by weight of oil-phase antioxidant to 20-40 parts by weight of oil, and heat and stir at 50-70°C until uniform; (3) mixing the liquids prepared in steps (1) and (2), emulsifying at 50-70°C, and then homogenizing at 50-70 MPa to complete the primary emulsification; (4) Add 80% of the weight of diglycerol to the liquid obtained in step (3), emulsify at 50-70°C, shear at 5000-8000 r / min for 2-5 min, homogenize at 20-40 MPa, complete secondary emulsification, and sterilize to obtain the final product.
2. The emulsion according to claim 1, characterized in that: The oil is at least one selected from soybean oil, sunflower oil, linseed oil, conjugated linoleic acid glyceride, medium-chain triglyceride, pumpkin seed oil, tomato seed oil, docosahexaenoic acid oil, eicosapentaenoic acid oil and animal fat; the amount of the oil added is 25-38 parts by weight.
3. The emulsion according to claim 1, characterized in that: The modified starch is sodium starch octenylsuccinate; the added amount of the modified starch is 7-13 parts by weight.
4. The emulsion according to claim 1, characterized in that: The diglyceride is selected from one of olive seed oil diglyceride oil, soybean oil diglyceride oil, linseed oil diglyceride oil, rapeseed oil diglyceride, safflower oil diglyceride, sunflower oil diglyceride and corn oil diglyceride oil, or a mixture of several of them.
5. The emulsion according to claim 1, characterized in that: The dietary fiber comprises one or a mixture of resistant dextrin, inulin, isomaltooligosaccharide, fructooligosaccharide, lacto-oligosaccharide, xylo-oligosaccharide, soybean oligosaccharide and polydextrose.
6. The emulsion according to claim 1, characterized in that: The small molecule sugar includes at least one of sucrose, glucose syrup, white sugar, glucose powder, lactose or maltose.
7. The emulsion according to claim 1, wherein: The osmotic pressure of the emulsion is 100-320 mOsm / kgH2O, and the emulsion remains uniform and stable after five freeze-thaw cycles without any demulsification or stratification, and has the inherent flavor of the product.
8. The method for preparing the emulsion according to claim 1, wherein: The steps include: (1) Disperse 5-15 parts by weight of modified starch in 80-120 parts by weight of water at 50-70°C, add 7-13 parts by weight of dietary fiber and 2-7 parts by weight of small molecule sugar, dissolve them, and adjust the osmotic pressure of the system to 100-250mOsm / kgH2O; then add 0-2 parts by weight of aqueous antioxidant, dissolve them, and adjust the osmotic pressure of the system to 100-320mOsm / kgH2O; (2) Add 20% by weight of diglyceride and 0-2 parts by weight of oil-phase antioxidant to 20-40 parts by weight of oil, and heat and stir at 50-70°C until uniform; (3) mixing the liquids prepared in steps (1) and (2), emulsifying at 50-70°C, and then homogenizing at 50-70 MPa to complete the primary emulsification; (4) Add 80% by weight of diglyceride to the liquid obtained in step (3), emulsify at 50-70°C, shear at 5000-8000 r / min for 2-5 min, homogenize at 20-40 MPa, complete secondary emulsification, and sterilize to obtain the final product.
9. Use of the low or isotonic antifreeze-thaw emulsion according to claim 1 in the food field, wherein the application includes the technical field of preparing beverages, prepared dairy products, yogurt, cheese, complementary foods, seasonings, and frozen desserts.
10. The use according to claim 9, characterized in that: The beverages include energy drinks, functional drinks, and fruit juices; the seasonings include sauces; and the frozen desserts include ice cream.
Citation Information
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