High-oil-loading microcapsule powder embedded with various polar oils, and formula, preparation method and application of high-oil-loading microcapsule powder

Abstract

The invention discloses a high-oil-loading microcapsule powder embedded with various polar oils, and a formula, a preparation method and application thereof, which are particularly suitable for efficient embedding of various polar oils, such as diglyceride, glycolipid, phospholipid and the like. By selecting the wall material, the emulsifying agent and the filling agent and optimizing the emulsifying process, the high oil carrying capacity is remarkably improved, and meanwhile the excellent heat-resistant stability and the low surface oil content are kept. The microcapsule powder not only has strong oxidation resistance, but also can maintain stable flavor during long-time storage, and is suitable for being applied to various foods and health care products, including but not limited to tablets, candies, bread baking and the like. And the method shows strong industrialization potential and wide applicability. The breakthrough provides a more reliable and efficient solution for the food industry, and the diversified market requirements are met.

Description

Technical Field

[0001] The present invention belongs to the technical field of microcapsule powder, and particularly relates to a high oil-loaded microcapsule powder with multiple polar oils embedded therein, its formulation, preparation method and application. Background Art

[0002] Generally speaking, the chemical composition of oils and fats is triacylglycerol, abbreviated as triglyceride. Its structure has three hydroxyl groups on glycerol, and it should form esters with three molecules of fatty acids to form non-polar triglycerides. However, in actual situations, not all hydroxyl groups on glycerol can be completely "esterified", and there will always be a small amount of hydroxyl groups without a partner, so there will be a small amount of diglyceride and monoglyceride in the oils and fats. These remaining hydroxyl groups are polar, making diglyceride a kind of polar oil. In addition, in addition to diglyceride, there are many other structures that make oils and fats polar. For example, phospholipids rich in oils and fats. Usually, we know that phospholipids are one of the main components of cell membranes. Its molecular structure contains a hydrophilic phosphate head and two hydrophobic fatty acid tails. This "head-tail" structure gives phospholipids strong amphiphilicity (that is, having both hydrophilic and hydrophobic properties at the same time), which is also the source of its polarity. Phospholipid oils, such as egg yolk oil, egg oil, phospholipid algal oil, krill oil rich in phospholipids, and many natural algal oils or deep-sea fish oils also contain a small amount of phospholipids and other polar lipids, making them also show certain polar characteristics as a whole. In addition, there are glycolipids. Glycolipids are a class of complexes that combine the characteristics of carbohydrates and lipids. They connect sugar chains with fatty acids or glycerol skeletons through glycosidic bonds. This unique structure makes the oils and fats containing glycolipids show a certain degree of polarity. For example, oat oil shows polarity because it contains water-soluble polysaccharides such as β-glucan and a certain amount of unsaturated fatty acids, making the intermolecular interactions more complex. The presence of these polar components not only enriches the biological functions of oils and fats, but also provides broad space for their applications in the fields of food, medicine and cosmetics.

[0003] Polar lipids currently face some challenges during the encapsulation and emulsification processes. Since polar lipids are hydrophilic, the wall material needs to be able to effectively encapsulate the polar lipids to prevent them from reacting with moisture or other components in the environment. In addition to emulsifying properties, the system also needs to have a certain degree of hydrophobicity and stability. If the polarity of the wall material is too low, it may not be able to effectively encapsulate krill oil, while if the polarity is too high, it may cause the encapsulated core material to be unstable during storage or use. Currently, the most commonly used method for preparing microcapsule powder is to first form an O / W emulsion system with various microcapsule wall materials and long-chain polyunsaturated fatty acids, and then use spray drying to prepare it. However, most of the current technologies on the market are more suitable for the encapsulation of conventional triglyceride types, that is, non-polar lipids, and the encapsulation of polar lipids is rare, especially for high-loading polar lipids. This is because to obtain a stable O / W system, emulsifiers often need to form a protective film at the oil-water interface. However, the high content of polar lipid core materials often causes the interfacial tension to decrease excessively, resulting in a weakening of the interaction force between the emulsion droplets, making the emulsion droplets prone to aggregation and over-emulsification, thus destroying the stability of the emulsion and making it difficult for the emulsifier to form a stable protective film at the oil-water interface. After demulsification, the water and oil in the emulsion will separate, and a stable O / W system cannot be formed. Therefore, the content of polar lipid products on the market is often low because higher oil loading means stronger polarity, and the hydrophilic core material is more likely to be released and dissolved, resulting in a high oil content on the product surface, poor stability, easy deterioration of the storage flavor, poor thermal stability, and difficulty in being applied to various scenarios.

[0004] In this case, how to obtain acid microcapsule powder with high oil loading, low surface oil, high thermal stability, good flavor, and applicable to a variety of polar oils through the optimization of preparation technical means is a difficult point that urgently needs to be solved. A series of research results on related polar oil microcapsule powder are recorded in the prior art: CN108003021B discloses such a technical solution: using soy lecithin-modified protein and maltodextrin to encapsulate diglyceride, and adding perilla extract to improve the product stability. The final diglyceride encapsulation rate is about 90-95%, and the peroxide value ≤ 8.0 meq / kg. CN118120829A discloses such a technical solution: mixing monoglyceride and diglyceride of rice bran oil to obtain an oil phase, and then mixing resistant dextrin, sodium caseinate and water for the second time to obtain an aqueous phase. Mix the oil phase and the aqueous phase, and after emulsification, homogenization and spray drying, obtain diglyceride of rice bran oil powder grease with low surface oil and good stability. CN201510150317.8 discloses such a technical solution: taking the main wall material, auxiliary wall material and emulsifier, stirring and dissolving to obtain an aqueous phase, adding an emulsifier to krill oil to obtain an oil phase, and then mixing the aqueous phase and the oil phase, shearing, homogenizing and spray drying to obtain the corresponding microcapsule, wherein the proportion of krill oil is 9.9%-30%. CN112040783A discloses such a technical solution: dissolving or dispersing carbohydrates, protein-containing powders and fats in water, and then spray drying the solution or dispersion to form a powder, or directly grinding to obtain the corresponding powder, and then coating the powder with glycolipid by spraying. Finally, a powdered beverage containing about 3.5-6% glycolipid and fat with a melting point higher than 20 °C is obtained. These patents have all disclosed methods for preparing corresponding microcapsule powder from various polar oils, such as diglyceride, phospholipid or glycolipid, but most of them may have the following limitations in practical applications. For example, chemical reagents are used in the modification process of the wall material protein, and the process is relatively complex, or the proportion of the core oil is relatively low. For example, the dosage of krill oil is only below 30%, and the proportion of glycolipid is only less than 6%. The low oil loading may limit the subsequent application fields of the product. In addition, some methods such as spraying may be difficult to achieve uniform coating of the core material, affecting the stability of the product. And currently, there are few embedding means and methods applicable to a variety of polar oils, and their oil loading is low, making it difficult to achieve the high oil loading and heat resistance stability effects in the present invention. Summary of the Invention

[0005] In order to solve the problems in the background art, the present invention aims to provide high oil-loaded microcapsule powder embedded with various polar oils, its formulation, preparation method and application. Considering subsequent production and practical application problems, the present invention selects specific combinations of raw and auxiliary materials and the addition sequence, and through the regulation of the HLB value of the emulsion phase and the selection and control of the emulsification process, microcapsule powder suitable for embedding various polar oils, such as diglycerides, glycolipids, phospholipids, etc., is obtained, and the obtained microcapsule powder has higher oil loading and good heat stability.

[0006] First, the present invention protects the formulation of high oil-loaded microcapsule powder embedded with various polar oils in the first aspect, which comprises the following components in parts by weight:

[0007] 20-70 parts by weight of polar oil, 5-16 parts by weight of protein-based wall material or starch-based wall material, 1-5 parts by weight of emulsifier, 10-60 parts by weight of small molecule carbohydrate filler, 0-4 parts by weight of antioxidant, 0-2 parts by weight of acid-base regulator, 1-3 parts by weight of aqueous phase stabilizer.

[0008] For the above technical solution, preferably, the polar oil is selected from diglyceride oil, phospholipid oil or glycolipid oil; more preferably, the diglyceride oil includes various plant diglyceride oils; such as linseed diglyceride oil, peanut diglyceride oil, corn diglyceride oil, rapeseed diglyceride oil, coconut diglyceride oil, palm diglyceride oil, rice diglyceride oil, soybean diglyceride oil, sunflower diglyceride oil, pumpkin seed diglyceride oil, tomato seed diglyceride oil, safflower diglyceride oil, perilla seed diglyceride oil (perilla seed diglyceride oil, perilla seed diglyceride oil), camellia seed diglyceride oil, high oleic sunflower diglyceride oil, seabuckthorn seed diglyceride oil, pumpkin seed diglyceride oil, pine nut diglyceride oil, seabuckthorn fruit diglyceride oil, peony seed diglyceride oil, walnut diglyceride oil, olive diglyceride oil, hemp seed diglyceride oil (cannabis seed diglyceride oil), wheat germ diglyceride oil, grape seed diglyceride oil, rapeseed diglyceride oil, palm diglyceride oil, silybum marianum seed diglyceride oil, etc. or a mixture of several of them; and a mixture of one or more of animal oil diglyceride oils (such as butter diglyceride oil, fish oil diglyceride oil, etc.); the phospholipid oil includes plant phospholipid oil; such as sunflower phospholipid, soybean phospholipid, etc., and animal phospholipid oil (such as krill oil, egg yolk oil, phospholipid algal oil, etc.); the glycolipid includes vegetable oil rich in glycolipid; such as oat oil, rice bran oil, etc.; the addition amount of the polar oil is preferably 20-70 parts by weight, more preferably 35-65 parts by weight; the most preferred range is 40-60 parts by weight.

[0009] For the above-described technical solution, preferably, the protein-based wall material is selected from one or a mixture of several of casein, sodium caseinate, whey protein, gelatin, milk protein, soy protein, pea protein, pumpkin protein, hemp protein, chickpea protein, barley protein, and milk powder; the addition amount of the protein-based wall material is preferably 5-16 parts by weight, more preferably 6-13 parts by weight, and most preferably 8-11 parts by weight.

[0010] For the above-described technical solution, preferably, the molecular weight of the protein-based wall material is 50-200 kDa, more preferably 70-130 kDa, and most preferably 90-120 kDa.

[0011] For the above-described technical solution, preferably, the starch wall material mainly refers to sodium octenyl succinate starch; the addition amount of the starch-based wall material is preferably 5-16 parts by weight, more preferably 6-13 parts by weight, and most preferably 8-11 parts by weight.

[0012] For the above-described technical solution, preferably, the emulsifier is selected from one or a mixture of several of mono- and diglycerol fatty acid esters, polyglycerol fatty acid esters, sucrose fatty acid esters, sodium stearoyl lactylate, and calcium stearoyl lactylate; the addition amount of the emulsifier is 1-5 parts by weight, more preferably 2-4.5 parts by weight, and most preferably 3-4 parts by weight.

[0013] For the above-described technical solution, preferably, the HLB value of the emulsifier is 6-16, more preferably 8-14, and most preferably 10-12.

[0014] For the above-described technical solution, preferably, the filler is selected from one or a mixture of several of glucose syrup, lactose, maltose, solid corn syrup, and maltodextrin; the addition amount of the filler is 10-60 parts by weight, more preferably 20-55 parts by weight, and most preferably 35-50 parts by weight.

[0015] For the above-described technical solution, preferably, the DE value of the filler is 40-80, more preferably 45-75, and most preferably 60-70.

[0016] For the above-described technical solution, preferably, the antioxidant is selected from one or a mixture of several of d-α tocopherol, dl-α tocopherol, mixed tocopherols, rosemary extract, phospholipids, butylated hydroxyanisole, antioxidant 264, and tert-butylhydroquinone. Further preferably, it is a mixture of one or several of mixed tocopherols, antioxidant 264, rosemary extract, phospholipids, or butylated hydroxyanisole; the addition amount of the antioxidant is 0-4 parts by weight; more preferably 0.2-2.0 parts by weight; most preferably 0.1-1.0 parts by weight.

[0017] The rosemary extract is prepared according to the "National Food Safety Standard Food Additive Rosemary Extract GB 1886.172-2016", which is a food additive rosemary extract produced from the stems and leaves of rosemary through processes such as solvent extraction or supercritical carbon dioxide extraction and refining. The extraction solvents are water, methanol, ethanol, acetone, and / or n-hexane, and the total antioxidant components (calculated as carnosic acid and carnosol) are ≥10%.

[0018] For the above-described technical solution, preferably, the aqueous phase stabilizer is selected from one or a mixture of several of sodium citrate, potassium citrate, sodium tripolyphosphate, sodium hexametaphosphate, sodium polyphosphate, disodium hydrogen phosphate, dipotassium hydrogen phosphate, sodium dihydrogen phosphate, and potassium dihydrogen phosphate, with sodium citrate being preferred. The addition amount of the aqueous phase stabilizer is 1-3 parts by weight; more preferably 1-2.5 parts by weight; most preferably 1.5-2 parts by weight.

[0019] For the above-described technical solution, preferably, the composition further includes 0-2 parts of an acid-base regulator. When the selected wall material in the composition is a starch-based wall material, the acid-base regulator is not added; when the selected wall material in the composition is a protein-based wall material, the acid-base regulator is added to control the pH value of the system within the range of neutral to weakly alkaline, with the pH value being 7-10, more preferably 7.5-9.5, and most preferably 8.0-9.0.

[0020] For the above-described technical solution, preferably, the acid-base regulation includes an acidic regulator and a basic regulator. Among them, the acidic regulator is selected from one or a mixture of several of citric acid, sulfuric acid, hydrochloric acid, phosphoric acid, and malic acid, with citric acid and phosphoric acid being preferred; the basic regulator is selected from one or a mixture of several of sodium hydroxide, sodium carbonate, potassium hydroxide, etc., with sodium hydroxide being preferred.

[0021] Another aspect of the present invention is to protect the microcapsule powder prepared using the above-described formula. The oil loading amount of the microcapsule powder is within the range of 20%-70%, which can not only ensure a good embedding effect but also avoid problems caused by too high or too low oil loading amounts.

[0022] Another aspect of the present invention is to protect a method for preparing a high oil-loaded microcapsule powder encapsulated with multiple polar oils using the formula described above, including steps such as raw material preparation, solution preparation, regulation of the HLB value of the emulsion phase, two-stage emulsification preparation of the emulsion, spray drying, etc., specifically the following steps:

[0023] (1) Fully dissolve the protein-based wall material or starch-based wall material and small molecule sugars in 80 - 150 parts by weight of water; when the wall material is a starch-based wall material, no acid-base regulator is added; when the wall material is a protein-based wall material, an acid-base regulator is added to control the pH value of the system within the range of neutral to weakly alkaline;

[0024] (2) Add the antioxidant to the polar oil;

[0025] (3) Add 50% of the total weight of the emulsifier to the liquid prepared in step (1);

[0026] (4) Mix the liquids prepared in steps (1) and (2), stir and shear, and homogenize and emulsify at a shear pressure of 40 - 60 MPa; where the stirring speed is 800 - 1000 rmp to obtain a primary emulsified emulsion, and more preferably the shear pressure is 45 - 55 MPa;

[0027] (5) Stir and disperse the remaining 50% of the total weight of the emulsifier and the aqueous phase stabilizer in the emulsion prepared in step (4);

[0028] (6) Homogenize the solution prepared in step (5) at 40 - 60 MPa to complete secondary emulsification, and more preferably the shear pressure is 45 - 55 MPa to obtain a secondary emulsified emulsion; perform spray drying to obtain the final product;

[0029] The last aspect of the present invention is to protect the application of the high oil-loaded microcapsule powder encapsulated with multiple polar oils in foods or health products.

[0030] Further preferably, the application includes fields such as tablets, powders, candies, gummies, soft capsules, bread baking, milk powder, yogurt, liquid beverages, solid beverages, energy bars, cheeses, complementary foods, various sauces, and ice creams.

[0031] Advantages of the present invention:

[0032] High oil loading and heat resistance stability

[0033] The microcapsule powder prepared by the present invention has a high oil loading of 20 - 70% and exhibits excellent heat resistance stability. After a 3-month accelerated stability test at 60°C, the appearance and water content of the product did not change significantly, and the surface oil, peroxide value, and acid value remained at low levels.

[0034] Overcoming the problem of embedding polar oils

[0035] The present invention solves the problem that a stable O / W system cannot be obtained during the embedding and emulsification of polar oils, avoids over-emulsification phenomenon, and achieves a stable microencapsulation effect.

[0036] Wide applicability

[0037] The present invention is applicable to a variety of polar oils (such as diglycerides, glycolipids, phospholipids, etc.), and can be adjusted according to different application requirements, expanding the application scenarios of the product. It can be widely used in tablets, powders, candies, gummies, soft capsules, bread baking, milk powder, yogurt, liquid beverages, solid beverages, energy bars, cheeses, complementary foods, various sauces, ice creams and other fields.

[0038] Improving the embedding efficiency

[0039] By optimizing the HLB value of the emulsifying phase and the two-stage emulsification process, the embedding efficiency of polar oils is significantly improved, ensuring a higher oil loading (20 - 80%), while maintaining the stability and uniformity of the microcapsule powder.

[0040] Improving the fluidity of the product

[0041] Selecting an appropriate ratio of wall material and filler makes the microcapsule powder have good fluidity, facilitating subsequent processing and packaging, and reducing losses and blockage problems during the production process.

[0042] Reducing the surface oil content

[0043] Controlling the surface oil content of the final product to ≤2% ensures a high embedding rate and low surface oil of the product, improving the sensory quality and application range of the product.

[0044] Enhancing the antioxidant performance

[0045] The antioxidant added to the formula effectively delays the oxidative degradation of polar oils, extends the shelf life of the product, especially showing outstanding performance under long-term storage conditions.

[0046] Improving the flavor stability of the product

[0047] The microcapsule powder maintains good flavor stability during long-term storage, avoiding the generation of off-flavors caused by oil oxidation, and improving the acceptance of consumers.

[0048] Simplifying the production process

[0049] The preparation method of the present invention simplifies the production process, reduces the operation steps and equipment requirements, lowers the production cost, while ensuring the consistency and stability of the product quality.

[0050] Environmentally friendly

[0051] During the preparation process, clean solvent ethanol was used and removed and recycled. The solvent residue in the product is less than 50 ppm, meeting the regulatory requirements of the food processing industry and causing no environmental pollution.

[0052] Strong industrial adaptability

[0053] The preparation method of the present invention has very good industrial adaptability, can meet the needs of large-scale production, and ensure the stability and consistency of product quality.

[0054] Solve market pain points

[0055] It solves the problems commonly existing in polar oil products on the market, such as low content, high surface oil, poor stability, easy deterioration of storage flavor, and poor thermal stability, and provides a better solution for the market. Specific embodiments

[0056] 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 any form of limitation to the content of the invention. Unless otherwise specified, the percentages in this specification are all mass percentages.

[0057] In the examples, the product performance of the samples was evaluated. First, each sample was sampled and divided into several parallel samples; to ensure the scientificity and credibility of the product performance evaluation, the same number of multiple sub-samples were randomly selected for each product, and the evaluation was carried out using the same test conditions and measurement techniques, and the performance was quantified and compared through statistical analysis (calculating the average value) of the obtained data.

[0058] The rosemary extract described in the examples was prepared in accordance with "GB 1886.172-2016 National Food Safety Standard Food Additive Rosemary Extract", which is a food additive rosemary extract produced from the stems and leaves of rosemary through processes such as solvent extraction or supercritical carbon dioxide extraction and refining. The extraction solvents are water, methanol, ethanol, acetone, and / or n-hexane, and the total antioxidant components (calculated as carnosic acid and carnosol) are ≥10%.

[0059] Example 1

[0060] Weigh 120 g of water into a 500 mL beaker, with the water temperature at 60 °C. Add 10 g of casein and 15.3 g of solid corn syrup to it. The average molecular weight of the casein used is 90 kDa, and the DE value of the solid corn syrup is selected as 65. Stir at 150 rmp until completely dissolved, and then adjust the pH of the emulsion to 8.5 with 0.1% concentration sodium hydroxide. This is the aqueous phase. Weigh another 70 g of linseed diglyceride, 0.2 g of mixed tocopherols and 1.5 g of glycerol monostearate citrate into a 200 mL beaker, heat in a water bath at 60 °C, and mix and stir evenly. The HLB value of the glycerol monostearate citrate is selected as 10. This is the oil phase. Pour the oil phase into the aqueous solution, stir at 60 °C, then stir at 9000 rmp for 40 minutes to complete the primary shearing, and then homogenize at 50 MPa to obtain the primary emulsified emulsion. Weigh another 1.5 g of sodium citrate and 1.5 g of glycerol monostearate citrate and add them to the emulsion. Stir at 150 rmp in a 70 °C water bath until completely dispersed, and then homogenize at 50 MPa to complete the secondary emulsification. Finally, spray-dry the obtained secondary emulsified emulsion, with the inlet air temperature at 180 °C and the outlet air temperature at 85 °C, to obtain the corresponding microcapsule powder. Screen and package the dried powder, and label it as sample 1.

[0061] Example 2

[0062] Weigh 150 g of water into a 500 mL beaker, with the water temperature at 60 °C. Add 8 g of sodium caseinate and 44 g of glucose syrup to it. The average molecular weight of the sodium caseinate used is 120 kDa, and the DE value of the glucose syrup is selected as 70. Stir at 150 rmp until completely dissolved, and then adjust the pH of the emulsion to 8.0 with 0.1% concentration potassium hydroxide. This is the aqueous phase. Weigh another 45 g of Antarctic krill oil, 0.02 g of antioxidant 264 and 1.0 g of sucrose fatty acid glyceride into a 200 mL beaker, heat in a water bath at 70 °C, and mix and stir evenly. This is the oil phase, and the HLB value of the sucrose fatty acid glyceride is selected as 16. Pour the oil phase into the aqueous solution, stir at 60 °C, then stir at 8000 rmp for 35 minutes to complete the primary shearing, and then homogenize at 40 MPa to obtain the primary emulsified emulsion. Weigh another 1.0 g of sucrose fatty acid ester and 1.0 g of sodium tripolyphosphate and add them to the emulsion. Stir at 150 rmp in a 65 °C water bath until completely dispersed, and then homogenize at 60 MPa to complete the secondary emulsification. Finally, spray-dry the obtained secondary emulsified emulsion, with the inlet air temperature at 180 °C and the outlet air temperature at 85 °C, and the inlet air temperature at 170 °C and the outlet air temperature at 75 °C, to obtain the corresponding microcapsule powder. Screen and package the dried powder, and label it as sample 2.

[0063] Example 3

[0064] Weigh 80 g of water into a 500 mL beaker. The water temperature is 60 °C. Add 11 g of sodium octenyl succinate starch and 50 g of maltodextrin to it. The DE value of the maltodextrin is selected as 50. Stir at 150 rmp until completely dissolved, and then adjust the pH of the emulsion to 7.0 with 0.1% calcium hydroxide and 0.1% citric acid. This is the aqueous phase. Then weigh 35 g of oat oil, 0.07 g of rosemary extract and 0.7 g of mono- and diglycerides of fatty acids into a 200 mL beaker. Heat in a water bath at 60 °C and mix and stir evenly. This is the oil phase. The HLB value of the mono- and diglycerides of fatty acids is selected as 6. Pour the oil phase into the aqueous solution, stir at 60 °C, then stir at 10,000 rmp for 30 minutes to complete the primary shearing, and then homogenize at 40 MPa to obtain the primary emulsified emulsion. Then weigh 0.7 g of mono- and diglycerides of fatty acids and 2.0 g of dipotassium hydrogen phosphate and add them to the emulsion. Stir at 150 rmp in a 65 °C water bath until completely dispersed, and then homogenize at 50 MPa to complete the secondary emulsification. Finally, spray-dry the obtained secondary emulsified emulsion. The inlet air temperature is 200 °C and the outlet air temperature is 90 °C to obtain the corresponding microcapsule powder. Then screen and package the dried powder, which is recorded as sample 3.

[0065] Example 1: Using casein as the wall material, glyceryl citrate fatty acid as the emulsifier, diglyceride of linseed oil as the fatty acid source, and mixed tocopherols as the antioxidant, after spray drying, a microcapsule powder of polar oil with an oil content of 70% is obtained.

[0066] Example 2: Using sodium caseinate as the wall material, sucrose fatty acid glyceride as the emulsifier, Antarctic krill oil as the fatty acid source, and antioxidant 264 as the antioxidant, after spray drying, a microcapsule powder of polar oil with an oil content of 45% is obtained.

[0067] Example 3: Using sodium octenyl succinate starch as the wall material, mono- and diglycerides of fatty acids as the emulsifier, oat oil as the fatty acid source, and rosemary extract as the antioxidant, after spray drying, a microcapsule powder of polar oil with an oil content of 35% is obtained.

[0068] Judging from the selection of wall materials, casein and sodium caseinate used in Examples 1 and 2 are proteins of animal origin, while the modified starch of plant origin is used in Example 3.

[0069] Judging from the selection of fatty acid sources, diglyceride of linseed oil used in Example 1 has a certain amount of polar diglyceride, Antarctic krill oil used in Example 2 has a phospholipid structure; oat oil used in Example 3 is rich in glycolipids.

[0070] Judging from the selection of antioxidants, mixed tocopherols and antioxidant 264 used in Examples 1 and 2 are both common food-grade antioxidants; while rosemary extract used in Example 3 is a natural antioxidant.

[0071] Example 4

[0072] Product performance evaluation was carried out on Sample 1, Sample 2 and Sample 3, and the long-term stirring stability test was carried out on the emulsion before spray drying. Due to the over-emulsification phenomenon of the polar oil solution, if the emulsion becomes unstable after stirring, the particle size will increase, and the emulsion will show water-oil stratification, etc., so that it cannot be applied in large-scale production. In addition, the measurement of the surface oil size of the microcapsule powder obtained after spray drying can intuitively show the product embedding rate. The lower the surface oil, the better the embedding property. Generally, it is considered that when the surface oil ≤ 2%, it has a good embedding property. The final results are shown in Table 1:

[0073] Table 1

[0074]

[0075] It can be seen from the results that the polar oil microcapsule powder obtained by the process disclosed in this application has good appearance, taste and smell, and the long-term stirring of the emulsion can ensure the stability of the emulsion, with the particle size D99 ≤ 5.0, and no demulsification or water-oil stratification phenomenon occurs after stirring for 24 hours. The surface oil is all ≤ 2%, and the embedding rate ≥ 98.0%, which proves that it has a firm embedding effect. This is related to the selection of specific raw and auxiliary materials and process steps in this preparation process, through the regulation of the HLB value of the emulsifying phase, the two-stage emulsification preparation of the emulsion, and the regulation of the spray drying parameters, to obtain a microcapsule powder with higher oil loading and good heat stability, which is applicable to a variety of polar oils. During the preparation process, the emulsion is stable during long-term stirring, can be scaled up for production, and this invention breaks through the essential problem of the unstable O / W system that cannot be obtained during the embedding and emulsification of polar oils, and the over-emulsification phenomenon occurs. It solves many problems such as low content of polar oil products on the market, high surface oil, poor stability, easy deterioration of storage flavor, poor heat stability, and difficulty in application in various scenarios. It can be widely used in tablets, powders, candies, gummies, soft capsules, bread baking, milk powder, yogurt, liquid beverages, solid beverages, energy bars, cheese, complementary foods, various sauces, and ice cream and other fields. The process can be scaled up for production and can avoid pollution by organic reagents, etc., which is environmentally friendly.

[0076] Example 5

[0077] Samples 1, 2 and 3 were respectively divided into several parallel samples; they were respectively placed in an accelerated oven at 40°C and 75% humidity for three months of product stability evaluation. The results are shown in Table 2:

[0078] Table 2

[0079]

[0080]

[0081] It can be seen from the accelerated stability test in a thermostatic and humidistatic chamber that after 3 months of acceleration, the appearance and water content of the three samples did not change significantly. In terms of taste and smell, there was no obvious fishy smell or rancid smell of grease. The surface oil, peroxide value and acid value increased slightly. Generally, it is considered that when the surface oil after three months of acceleration is ≤5%, the peroxide value is ≤10.0 meq / kg, and the acid value is ≤1.0 mgKOH / g, the thermal stability of the product is better. It can be seen that the product prepared by the process of this application has dense embedding, excellent heat resistance, antioxidant stability and storage stability.

[0082] Example 6

[0083] Based on the process of Example 1, without changing the original formula materials and their proportions, only the HLB value of the emulsifier is changed. The influence of the HLB value of the emulsifier on the stability of the emulsion prepared from polar oil and the influence on the state of the microcapsule powder formed by subsequent spray drying are mainly investigated. The product state is shown in Table 3:

[0084] Table 3

[0085]

[0086]

[0087] From the results, based on the process of Example 1, adjusting the HLB value of the emulsifier will significantly affect the product performance of the microcapsule powder. Whether the HLB value is too large or too small, it will lead to a decrease in the stirring stability of the emulsion, obvious increase in particle size, oil floating or even emulsion breaking, and ultimately result in the failure of microcapsule powder preparation or a decrease in product quality. For the samples with the HLB value in the range of 6 - 16, the surface oil is lower. The destructive stability investigation experiment of the emulsion is carried out by stirring for 5 - 24 h respectively. No obvious oil floating occurs in the emulsion, the particle size D99 ≤ 5.0, and the product is qualified, and it can be used for long-term continuous production at industrial scale. Therefore, the HLB value of the emulsifier must be controlled within the range of 6 - 16 to achieve the corresponding emulsion stability effect and obtain microcapsule powder with low surface oil and dense embedding.

[0088] Example 7

[0089] Based on the process of Example 1, without changing the original formula materials and their proportions, the emulsification process is changed. The influence of the emulsification process of the emulsion twice on the product performance is mainly investigated. The product state is shown in Table 4:

[0090] Table 4

[0091]

[0092]

[0093] Judging from the results, the number of emulsification times for preparation must be 2 times. If it is less than 2 times, the emulsification effect cannot be achieved. After homogenization, the particle size of the emulsion is relatively large, the surface oil content increases significantly, and the particle size increases significantly after the emulsion is stirred for 24 hours, with a large amount of oil floating. When the number of emulsification times is higher than 2 times, such as 4 times, demulsification occurs directly. For 3 times of emulsification, the particle size of the emulsion is relatively small at the beginning, but soon the overly small oil droplets are prone to Ostwald ripening, and the emulsion becomes unstable subsequently, and the surface oil content of the product is also relatively high. Therefore, the number of emulsification times for preparation must be 2 times to achieve the corresponding emulsion stability and embedding effect.

[0094] Example 8

[0095] Based on the process of Example 1, without changing the original formula materials and their proportions, the molecular weight of the protein-based wall material is adjusted, and the effect of the molecular weight of the protein-based wall material on the sample state is mainly investigated. The test results are shown in Table 5:

[0096] Table 5

[0097]

[0098] Judging from the results, the surface oil content of Samples 1 and 2 is relatively low, and the emulsion stability is good. As the average molecular weight of the protein-based wall material decreases, the surface oil content also increases accordingly. In addition, when the average molecular weight of the protein-based wall material is too large, the viscosity of the powder will also increase, resulting in an increase in the particle size of the emulsion after obvious homogenization. The average molecular weight of the protein-based wall material must be in the range of 50 - 200 kDa. If it is less than 50 kDa, the protein-phase emulsion is relatively dilute, the particle size is too small just after homogenization, then Ostwald ripening occurs, and floating oil is likely to occur during the final stirring process, such as in Comparative Examples 10 - 11, and the surface oil content of the product obtained by spray drying is relatively high. When the molecular weight is greater than 200 kDa, the viscosity is too high and the emulsion particle size is too large, which will also affect the final embedding effect, such as in Comparative Examples 13 - 15. The detected surface oil of all of them is greater than 5%, and the products are unqualified. Therefore, if a protein-based wall material is selected, the average molecular weight of the protein must be in the range of 50 - 200 kDa (the best is 70 - 130 kDa), which can ensure that the product has a good embedding effect, while maintaining a low surface oil content and achieving the corresponding emulsion stability effect to adapt to large-scale production.

[0099] Example 9

[0100] Based on the process of Example 1, without changing the original formula materials and their proportions, the DE value of the filler is adjusted, and the effect of the DE value on the sample state is mainly investigated. The test results are shown in Table 6:

[0101] Table 6

[0102]

[0103] Judging from the results, the DE value of the filler has a certain impact on the sample state. As the DE value of the filler increases, the surface oil of Samples 1, 2, and 3 significantly differs. When sugars with too low DE values (such as Comparative Examples 17-19) are dissolved, the viscosity is too high, the filling effect is poor, and pores are likely to appear. While fillers with higher DE values ≥ 90 (such as Comparative Example 22) are prone to caking and moisture absorption after spray drying, the powder is sticky, and the Ostwald ripening phenomenon is also likely to occur in the emulsion. The initial emulsion particle size is very small and becomes unstable after stirring. Samples with filler DE values in the range of 40-80 have better powder states. The further preferred DE value is 45-75, and the optimal DE value is 60-70, and the surface oil is all ≤ 2.0%, the product is qualified, and the emulsion is stable.

[0104] Example 10

[0105] Based on the process of Example 1, without changing the original formula materials and proportions, the oil loading amount was adjusted, and the impact of the oil loading rate on the sample state was mainly investigated. The test results are shown in Table 7:

[0106] Table 7

[0107]

[0108] Judging from the results, too high or too low oil loading amounts have a certain impact on the sample state. As the oil loading amount of the filler decreases, such as in Comparative Examples 24-25, the tower adhesion is serious during the powder spray drying and collection processes, and a wire-drawing state appears. Although the surface oil is low, the product appearance is unqualified. While when the oil loading amount is too high, such as in Comparative Examples 26-18, the surface oil significantly increases, the powder is slightly sticky, and the state is poor and unqualified. Therefore, samples with oil loading amounts in the range of 20-70 have better powder states, and the surface oil is all ≤ 2.0%, and the product is qualified.

[0109] The above is only a preferred specific embodiment of the present invention, but the protection scope of the present invention is not limited thereto. Changes or substitutions that can be easily thought of by those skilled in the art within the technical scope disclosed by the present invention should all be covered within the protection scope of the present invention. Therefore, the protection scope of the present invention should be subject to the protection scope of the claims.

Claims

1. A formula for high oil-loaded microcapsule powder embedded with multiple polar oils, characterized in that: It comprises the following components by weight: 20 - 70 parts by weight of polar oil, 5 - 16 parts by weight of protein - based wall material or starch - based wall material, 1 - 5 parts by weight of emulsifier, 10 - 60 parts by weight of small - molecule sugar filler, 0 - 4 parts by weight of antioxidant, 0 - 2 parts by weight of acid - base regulator, and 1 - 3 parts by weight of aqueous - phase stabilizer.

2. The formulation according to claim 1, characterized in that: The polar oil is selected from diglyceride oil, phospholipid oil or glycolipid oil; the diglyceride oil includes plant diglyceride oil and animal diglyceride oil; the phospholipid oil includes plant phospholipid oil and animal phospholipid oil; the glycolipid includes vegetable oil rich in glycolipid.

3. The formulation according to claim 1, wherein: The protein - based wall material is selected from one or a mixture of casein, sodium caseinate, whey protein, gelatin, milk protein, soy protein, pea protein, pumpkin protein, hemp protein, chickpea protein, barley protein, milk powder.

4. The formulation according to claim 1, wherein: The molecular weight of the protein - based wall material is 50 - 200 kDa; the starch wall material is sodium octenyl succinate starch; the emulsifier is selected from one or a mixture of mono - and diglycerol fatty acid esters, polyglycerol fatty acid esters, sucrose fatty acid esters, sodium stearoyl lactate, calcium stearoyl lactate.

5. The formulation according to claim 1, wherein: The HLB value of the emulsifier is 6 - 16.

6. According to the formulation of claim 1, it is characterized in that: The filler is selected from one or a mixture of glucose syrup, lactose, maltose, solid corn syrup, maltodextrin; the DE value of the filler is 40 - 80.

7. The formulation according to claim 1, wherein: The aqueous - phase stabilizer is selected from one or a mixture of sodium citrate, potassium citrate, sodium tripolyphosphate, sodium hexametaphosphate, sodium polymetaphosphate, disodium hydrogen phosphate, dipotassium hydrogen phosphate, sodium dihydrogen phosphate, potassium dihydrogen phosphate.

8. High-loaded oil microcapsule powder embedded with multiple polar oils prepared by using the formula described in claim 1, characterized in that: The oil - loading amount of the microcapsule powder is 20% - 70%.

9. Preparation method of high oil-loaded microcapsule powder embedded with multiple polar oils, characterized in that: It includes the following steps: (1) Dissolve the protein - based wall material or starch - based wall material and small - molecule sugar fully in 80 - 150 parts by weight of water; when the wall material is starch - based wall material, no acid - base regulator is added; when the wall material is protein - based wall material, an acid - base regulator is added to control the pH value of the system within the range of neutral to weakly alkaline. (2) Add the antioxidant to the polar oil. (3) Add 50% of the total weight of the emulsifier to the liquid prepared in step (1). (4) Mix the liquids prepared in steps (1) and (2), stir and shear, and homogenize and emulsify at a shear pressure of 40 - 60 MPa. Obtain the primary emulsified emulsion. (5) Stir and disperse the remaining 50% of the total weight of the emulsifier and the aqueous - phase stabilizer fully in the emulsion prepared in step (4). (6) Homogenize the solution prepared in step (5) at 40 - 60 MPa to complete the secondary emulsification, and perform spray drying to obtain the final product.

10. Use of the high - oil - loading microcapsule powder encapsulated with multiple polar oils as described in claim 1 in food or health products.

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