High-stability multivitamin mineral microgel carrier and preparation method thereof
By preparing solutions of water-soluble and oil-soluble vitamins and minerals and cross-linking them to form microgels, the stability problem of vitamins and minerals during storage and heating in the existing technology is solved, and the stable encapsulation and protection of multiple vitamins is achieved, which is suitable for applications in multiple scenarios.
Patent Information
- Application Number
- CN202510939409.8
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-07-08
- Publication Date
- 2025-09-26
AI Technical Summary
Existing vitamin and mineral nutritional supplements have poor stability during storage and heating, making it difficult to simultaneously encapsulate multiple water-soluble and oil-soluble vitamins. In addition, the preparation process is complex, making them difficult to use for people with swallowing disorders.
By preparing a solution containing water-soluble and oil-soluble vitamins and minerals, using polysaccharides to cross-link under appropriate conditions to form microgels, and shearing them into microgels, the process is simplified and stability is maintained.
It achieves stable encapsulation and protection of multiple vitamins and minerals, is suitable for application in multiple scenarios, especially for people with dysphagia, and has a simple preparation process.
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Figure CN120694403A_ABST
Abstract
Description
Technical Field
[0001] The present invention belongs to the field of functional foods and nutritional products, and particularly relates to a functional microgel loaded with multiple vitamins / minerals and a preparation method thereof. Background Art
[0002] Vitamins and minerals are essential nutrients for the human body and play an irreplaceable role in maintaining human health and normal physiological functions. Vitamins and minerals can be obtained from natural foods. However, with the evolution of lifestyle and changes in dietary structure, ultra-processed foods based on fine processing and deep processing have gradually become the main component of human food intake, and excessive cooking methods have also become mainstream. As a result, the original vitamins and minerals in the food often undergo serious structural damage or loss of content during the processing process. Daily intake alone is no longer able to meet the body's demand for vitamins and minerals. Timely and appropriate supplementation of multiple vitamins and minerals is very important for maintaining the body's metabolism and functional expression.
[0003] Vitamins and minerals have poor stability in aqueous solutions and are prone to physical system instability, chemical structure degradation or oxidation during storage and heat sterilization, resulting in reduced product performance. Therefore, current vitamin and mineral nutritional supplements are mainly solid composite products such as tablets and capsules. However, solid products have certain limitations in actual use and are difficult to use in elderly people or related patient groups with chewing and swallowing difficulties. Semi-solid and liquid products such as soft candies and oral liquids only carry a relatively single type of vitamins or minerals, making it difficult to simultaneously encapsulate and protect multiple water-soluble vitamins, oil-soluble vitamins, and minerals.
[0004] A Chinese invention patent application (publication number CN 106821998 B) discloses a vitamin AD micropill prepared using gelatin and sucrose. However, the micropill uses multiple processing steps, including spray drying and freeze drying, and contains only a few types of vitamins, resulting in poor nutritional efficacy.
[0005] A Chinese invention patent application (publication number CN 117678751 A) discloses an oligosaccharide pectin gel loaded with a fat-soluble active ingredient. However, this gel only loads a single fat-soluble substance and requires the addition of gelling agents such as gluconolactone and oligosaccharides. The preparation process also involves a lengthy ultrasound step, making it cumbersome. Furthermore, the pectin gel formed by gluconolactone undergoes irreversible morphological collapse after thermal processing, making it difficult to sterilize in industrial production.
[0006] Currently, there is no multivitamin and mineral supplement on the market that can withstand storage and heating, has a soft texture and good fluidity. Summary of the Invention
[0007] The purpose of the present invention is to solve the problems of existing process technologies and to provide a method for preparing microgels with a gentle and simple technical route that can achieve the simultaneous encapsulation and protection of multiple vitamins / minerals. The present invention first prepares a solution containing water-soluble and oil-soluble vitamins, minerals, and liquid oil, and then uses a polysaccharide that can form a gel to mix with the above solution under appropriate conditions and cross-link to form a gel, and finally shears and crushes it into microgels to obtain the finished product. The microgel containing vitamins / minerals prepared by the present invention can significantly increase the vitamin retention content of the corresponding vitamin aqueous solution in a variety of processing scenarios, and the production process is simple, which is suitable for the development and application of complex vitamin and mineral products.
[0008] The purpose of the present invention is achieved by at least one of the following technical solutions.
[0009] The invention provides a microgel containing vitamins and minerals. Calculated by the mass of the final product, in addition to H2O, the microgel further comprises the following components: 0.05-1wt% of polysaccharide 1, 1.2-14wt% of polysaccharide 2, 0.5-1.5wt% of complex minerals, 0.3-0.5wt% of complex vitamins, and 0.4-1wt% of liquid oil.
[0010] Preferably, the polysaccharide 1 is one or more of sodium carboxymethyl cellulose, sodium methyl cellulose, gum arabic, soybean polysaccharide, pectin, citrus fiber, chitosan, and xanthan gum;
[0011] Preferably, the polysaccharide 2 is one or more of low methoxy pectin, amidated low methoxy pectin, beet pectin, curdlan gum, tamarind gum, and sodium alginate;
[0012] Preferably, the composite mineral is one or more of inorganic and / or organic salts of sodium, potassium, calcium, chlorine, magnesium, phosphorus, iodine, iron, manganese, zinc, copper and selenium;
[0013] Preferably, sodium is used in the form of sodium citrate and / or sodium chloride, potassium is used in the form of potassium chloride and / or potassium iodide, calcium is used in the form of calcium carbonate and / or tricalcium phosphate, chlorine is used in the form of sodium chloride and / or potassium chloride, magnesium is used in the form of magnesium sulfate and / or oxidase, phosphorus is used in the form of tricalcium phosphate, iodine is used in the form of potassium iodide, iron is used in the form of ferric pyrophosphate, manganese is used in the form of manganese sulfate, zinc is used in the form of zinc gluconate, copper is used in the form of copper sulfate, and selenium is used in the form of sodium selenite;
[0014] Preferably, the vitamin complex is one or more of water-soluble vitamins and oil-soluble vitamins;
[0015] The water-soluble vitamins are one or more of vitamin B1, vitamin B2, vitamin B6, vitamin B12, niacin, folic acid, pantothenic acid, vitamin C and biotin; and the oil-soluble vitamins are one or more of vitamin A, vitamin D3, vitamin E and vitamin K1.
[0016] Preferably, vitamin B1 is used in the form of thiamine nitrate, vitamin B2 is used in the form of riboflavin, vitamin B6 is used in the form of pyridoxine hydrochloride, vitamin B12 is used in the form of cyanocobalamin, niacin is used in the form of niacinamide, pantothenic acid is used in the form of D-calcium pantothenate, vitamin C is used in the form of L-ascorbic acid; vitamin A is used in the form of vitamin A acetate, vitamin E is used in the form of dl-α-tocopheryl acetate, and vitamin K1 is used in the form of phytonadione.
[0017] Preferably, the liquid oil is one or more of sunflower oil, corn oil, soybean oil, rapeseed oil, peanut oil, olive oil, fish oil, algae oil, perilla oil, linseed oil, chia seed oil, medium chain triglycerides, and diglycerides;
[0018] Preferably, the microgel containing vitamins and minerals is characterized by comprising the following steps:
[0019] Step 1. Preparation of vitamin / mineral emulsion: shearing multivitamins, multiminerals, liquid oil, polysaccharide 1 with an appropriate amount of water to obtain a vitamin / mineral emulsion;
[0020] Step 2. Preparation of polysaccharide 2 aqueous solution: dissolving polysaccharide 2 in an appropriate amount of water with stirring to obtain a fully hydrated polysaccharide 2 solution;
[0021] Step 3. Formation of microgel: The polysaccharide 2 aqueous solution is mixed with the vitamin and mineral emulsion, kept at a certain temperature for a certain time, and then sheared to form a microgel.
[0022] Preferably, the shear rate in step 1 is 5000-10000 rpm, and the shear time is 1-2 min.
[0023] Preferably, the stirring rate in step 2 is 300 rpm, and the stirring time is 1-2 h.
[0024] Preferably, the insulation temperature in step 3 is 20-90° C., and the insulation time is 2-5 minutes.
[0025] Preferably, the shear rate in step 3 is 3000-6000 rpm, and the shear time is 0.5-1 min.
[0026] The microgel containing vitamins and minerals of the present invention has the following characteristics: after being subjected to treatments such as heating and storage, it can still maintain a stable macroscopic appearance and a high vitamin content.
[0027] The vitamin / mineral-containing microgel according to claim 1 can be suitable for one or more application scenarios of direct administration, administration after dilution, and processing after dilution in food and beverages, RTD nutritional health products, sports nutrition foods, and liquid special medical foods.
[0028] The present invention features a simple preparation process, readily available raw materials, and can effectively encapsulate and stabilize complex vitamins and minerals. It exhibits stability under conditions such as pasteurization, room-temperature storage, and water-soluble dilution, maintaining a stable macroscopic appearance and providing excellent protection for a variety of water-soluble and oil-soluble vitamins. The microgel of the present invention achieves multiple encapsulation and protection of minerals, water-soluble, and oil-soluble vitamins, exhibiting excellent stability and fluidity. Compared to tablet or capsule vitamin and mineral supplements, it offers improved swallowability and multi-scenario applicability. Furthermore, the preparation process is simple and mild, making it suitable for large-scale production and application.
[0029] Compared with the prior art, the advantages of the present invention also include:
[0030] 1. The vitamin / mineral microgel of the present invention utilizes the complex action of polysaccharide 1 having emulsifying properties and polysaccharide 2 capable of forming a gel. This allows minerals that are prone to sedimentation loss in aqueous solutions to be uniformly and stably dispersed in the gel system, while also allowing water-soluble and oil-soluble vitamins to be stably present in the aqueous and oil phases, respectively.
[0031] 2. The vitamin / mineral-containing microgel of the present invention has an absolute negative potential of 15-30 mV and an average particle size of 0.4-1.5 μm. The appearance and structure of the vitamin / mineral-containing microgel of the present invention are stable after storage and heat treatment.
[0032] 3. Compared with corresponding vitamin and mineral aqueous solutions, the vitamin / mineral microgel of the present invention has a better vitamin protection effect and can effectively reduce the loss rate of vitamins during storage and heating;
[0033] 4. The vitamin / mineral-containing microgels of the present invention have a simple and easy preparation process, which can be obtained through simple steps such as dissolution, mixing, and shearing. The process of the present invention can adjust the vitamin and mineral content and microgel volume according to the application scenario, providing multiple technical solutions for their application in the fields of food, beverages, health products, etc. BRIEF DESCRIPTION OF THE DRAWINGS
[0034] Figure 1 、 Figure 2 、 Figure 3 、 Figure 4 、 Figure 5 and Figure 6 These are micrographs of microgel 3, microgel 8, microgel 13, microgel 23, and microgel 28 prepared according to the embodiments of the present invention. DETAILED DESCRIPTION
[0035] In order to further understand the present invention, preferred embodiments of the present invention are described below in conjunction with examples, but it should be understood that these descriptions are only for further illustrating the features and advantages of the present invention, rather than for limiting the claims of the invention. Those skilled in the art can refer to the content of the present invention and appropriately improve the process parameters for implementation. It is particularly important to point out that all similar replacements and modifications are obvious to those skilled in the art, and they are all considered to be included in the present invention. The methods and applications of the present invention have been described through preferred embodiments, and relevant personnel can obviously modify or appropriately change and combine the methods and applications described in the present invention without departing from the content, spirit and scope of the present invention to implement and apply the technology of the present invention. Although it is believed that those of ordinary skill in the art fully understand the following terms, the following definitions are still stated to help illustrate the subject matter disclosed by the present invention.
[0036] As used herein, the term "comprising" is synonymous with "including," "containing," or "characterized by," and is inclusive or open-ended and does not exclude additional unrecited elements or method steps. "Comprising" is a technical term used in claim language to mean that the recited elements are present, but other elements may be added and still form a structure or method within the scope of the claim.
[0037] As used herein, "polysaccharide" refers to a molecule formed by the dehydration polymerization of multiple monosaccharide molecules, connected by glycosidic bonds, to form linear or branched long chains. Polysaccharides may include, but are not limited to, one or more of low-methoxyl pectin, amidated low-methoxyl pectin, beet pectin, gum arabic, soybean polysaccharide, citrus fiber, curdlan gum, tamarind gum, and sodium alginate. In the present invention, the weight of the polysaccharide, based on the weight of the microgel, is 1.2-15 wt%, for example, 1.2 wt%, 2 wt%, 3 wt%, 4 wt%, 5 wt%, 6 wt%, 7 wt%, 8 wt%, 9 wt%, 10 wt%, 11 wt%, 12 wt%, 13 wt%, 14 wt%, 15 wt%, or any range or value therebetween.
[0038] As used herein, "complex minerals" refers to compounds or natural elements that are essential to the human body but cannot be produced or synthesized independently, and are nutrients that exist primarily in the form of inorganic salts in the human body. Complex minerals are one or more inorganic and / or organic salts of sodium, potassium, copper, magnesium, iron, zinc, manganese, calcium, phosphorus, iodine, chlorine, and selenium. In the present invention, the content of complex minerals is 0.5-1.5 wt%, based on the weight of the microgel, for example, 0.5 wt%, 0.6 wt%, 0.7 wt%, 0.8 wt%, 0.9 wt%, 1 wt%, 1.1 wt%, 1.2 wt%, 1.3 wt%, 1.4 wt%, 1.5 wt%, or any range or point value therebetween.
[0039] As used herein, "complex vitamins" refers to a class of trace organic substances necessary for humans and animals to maintain normal physiological functions. Vitamins are further divided into water-soluble vitamins and oil-soluble vitamins based on their solubility. Water-soluble vitamins include one or more of vitamin B1, vitamin B2, vitamin B6, vitamin B12, niacin, folic acid, pantothenic acid, vitamin C, and biotin, and oil-soluble vitamins include one or more of vitamin A, vitamin D, vitamin E, and vitamin K1. In the present invention, the content of the complex vitamins is 0.3-0.5wt% based on the weight of the microgel, for example, 0.3wt%, 0.35wt%, 0.4wt%, 0.45wt%, 0.5wt%, or any range or point value therebetween.
[0040] As used herein, "liquid oil" refers to an oil in a fluid state, such as an oil that is fluid at room temperature. The liquid oil may include, but is not limited to, one or more of sunflower oil, corn oil, soybean oil, rapeseed oil, peanut oil, olive oil, fish oil, algae oil, perilla oil, linseed oil, chia seed oil, medium-chain triglycerides, and diglycerides. In the present invention, the liquid oil content is 0.4-1 wt %, for example, 0.4 wt %, 0.5 wt %, 0.6 wt %, 0.7 wt %, 0.8 wt %, 0.9 wt %, 1 wt %, or any range or value therebetween, based on the weight of the microgel.
[0041] The microgel of the present invention may or may not contain other ingredients besides the polysaccharide, complex minerals, complex vitamins, and liquid oil. Preferably, the microgel containing vitamins and minerals of the present invention does not contain other ingredients. Other ingredients may include, but are not limited to, gelatin, stabilizers, thickeners, or emulsifiers.
[0042] As used herein, "apparent viscosity" refers to the quotient obtained by dividing the corresponding shear stress by the shear rate under a given velocity gradient. Apparent viscosity is used only to roughly compare fluidity and includes reversible, highly elastic deformation. Apparent viscosity can be further divided into shear viscosity and extensional viscosity. Apparent viscosity may be greater or less than true viscosity.
[0043] As used herein, "zeta potential" refers to the amount of charge on the surface of a particle and is related to the stability of the particle system. The positive or negative value of the zeta potential depends on the composition of the system. Generally speaking, the higher the absolute value of the zeta potential, the greater the electrostatic repulsion between particles and the better the physical stability.
[0044] As used herein, "particle size" describes the size of a particle. When a physical property or behavior of a measured particle is most similar to that of a homogeneous sphere (or combination) of a certain diameter, the diameter of that sphere (or combination) is taken as the equivalent particle size (or particle size distribution) of the measured particle. "Average particle size" is a physical measure that represents the geometric size of a group of dispersed solid particles.
[0045] As used herein, "PDI" is a dimensionless value reflecting the width of the particle size distribution, indicating the degree of dispersion of the polymer, ranging from 0 to 1. The smaller the value, the more uniform the particle size and the more concentrated the particle size distribution.
[0046] Product preparation method
[0047] The vitamin- and mineral-containing microgels of the present invention can be prepared by mixing a gelling polysaccharide solution with a vitamin-mineral solution and, depending on the properties of the gelling polysaccharide, inducing gelation by heat or metal salts in the minerals. For gelling polysaccharides, the polysaccharide solution can be obtained by fully dissolving and hydrating the solution under magnetic stirring for 1-2 hours. The vitamins, minerals, and liquid oil are then shear-homogenized with water and mixed with the polysaccharide solution. The solution is then incubated at 20-90°C for 2-5 minutes before shearing to form the microgel. Incubation can be at or above room temperature for a period of time, such as at 20°C, 30°C, 40°C, 50°C, 60°C, 70°C, 80°C, 90°C, or higher, for 2 minutes, 3 minutes, 4 minutes, or 5 minutes, or any range or point therebetween.
[0048] Example
[0049] The embodiments of the present application will be described in detail below with reference to the examples, but it will be appreciated by those skilled in the art that the following examples are merely illustrative of the present application and should not be construed as limiting the scope of the present application. Specific conditions not specified in the examples are carried out according to conventional conditions or manufacturer recommendations. Reagents or instruments not specified in the manufacturer are conventional products commercially available. Unless otherwise indicated, all amounts listed are described in terms of weight percentage based on the total weight of the microgel (except for the mass percentage of each component, the remainder is water). The present application should not be construed as being limited to the specific examples described.
[0050] 1. Preparation Method
[0051] Step 1: preparing a solution containing 0.05-1 wt% of polysaccharide 1, 0.5-1.5 wt% of complex minerals, 0.3-0.5 wt% of complex vitamins, and 0.4-1 wt% of liquid oil, and shearing the solution at 8000 rpm for 2 minutes in an appropriate amount of water to obtain a vitamin and mineral solution;
[0052] Among them, every 100mg of complex minerals includes: Sodium (sodium citrate, sodium chloride) 25mg, Potassium (potassium chloride, potassium iodide, dipotassium hydrogen phosphate) 16.8mg, Calcium (calcium carbonate, tricalcium phosphate) 10mg, Chloride (sodium chloride, potassium chloride) 15mg, Magnesium (magnesium sulfate, oxidase) 3.2mg, Phosphorus (tricalcium phosphate, ferric pyrophosphate, dipotassium hydrogen phosphate) 7mg, Iodine (potassium iodide) 2μg, Iron (ferric pyrophosphate) 220μg, Manganese (manganese sulfate) 25μg, Zinc (zinc gluconate) 100μg, Copper (copper sulfate) 10μg, Selenium (sodium selenite) 0.75μg;
[0053] Among them, every 100mg of complex vitamins includes: Vitamin B10.425 mg, Vitamin B20.425 mg, Vitamin B60.35 mg, Vitamin B 12 0.85μg, niacin 1.4mg, folic acid 56μg, pantothenic acid
[0054] 1.4mg, vitamin C 70mg, biotin 3.5μg; vitamin A 130μg RE, vitamin D 2.5μg, vitamin E2.5mgα-TE, vitamin K110μg.
[0055] Step 2: 1.2-14 wt% polysaccharide 2 is prepared into an aqueous solution, and fully hydrated under magnetic stirring at 300 rpm for 1-2 hours to obtain a polysaccharide 2 solution;
[0056] Step 3: The above vitamin and mineral solution is mixed with the polysaccharide solution, kept at 20-90° C. for 2-5 minutes, and then sheared at 5000 rpm for 30 seconds to obtain a microgel containing vitamins and minerals.
[0057] 2. Test Method
[0058] ①Apparent viscosity
[0059] Instrument used: Anton Paar ViscoQC rotational viscometer
[0060] Test steps: Use an appropriate rotor to analyze the apparent viscosity of the microgel. After installing the rotor, place the measuring head of the rotor completely into the microgel and measure for 1 minute, and record the apparent viscosity value.
[0061] ②Average particle size, PDI and zeta potential
[0062] Instrument used: Nano ZS nanoparticle size and zeta potential analyzer
[0063] Testing steps: After the microgels were diluted in water at an appropriate multiple, the average particle size, PDI, and zeta potential of the microgels were measured.
[0064] ③ Vitamin content
[0065] Refer to GB14754-2010 National Food Safety Standard Food Additive Vitamin C (Ascorbic Acid), GB5009.82-2016 National Food Safety Standard Determination of Vitamins A, D, and E in Foods, and GB5009.296-2023 National Food Safety Standard Determination of Vitamin D in Foods.
[0066] Example 1
[0067] A microgel containing vitamins and minerals, the preparation method of which comprises the following steps:
[0068] (1) 0.5 wt% of arabic gum, 1.5 wt% of composite minerals, 0.5 wt% of composite vitamins, and 1 wt% of sunflower oil (the same below) were added to an appropriate amount of water, magnetically stirred at 300 rpm, and sheared at 8000 rpm for 2 min to obtain a vitamin and mineral solution;
[0069] (2) 1.2 wt%, 1.4 wt%, 1.6 wt%, 1.8 wt%, and 2.0 wt% of the final product mass of amidated low-methoxy pectin were uniformly dispersed in water, and fully hydrated under magnetic stirring at 300 rpm for 1-2 h to obtain amidated low-methoxy pectin solutions of different masses;
[0070] (3) Five portions of amidated low-methoxyl pectin solution of different masses obtained in step (2) were uniformly dispersed in the vitamin and mineral solution obtained in step (1), and the mixture was kept at 80° C. for 2 minutes to form a gel. Subsequently, the mixture was sheared at 5000 rpm for 30 seconds to obtain a microgel containing vitamins and minerals. The microgels containing vitamins and minerals obtained in this example were numbered as follows:
[0071] Table 1
[0072]
[0073] The term "whether it can be formed" in the table refers to whether it can form a gel with a certain elasticity, rather than a suspension dispersion system with a certain viscosity formed by the introduction of various components (the same below).
[0074] Example 2
[0075] A microgel containing vitamins and minerals, the preparation method of which comprises the following steps:
[0076] (1) 0.5 wt% of arabic gum, 1.5 wt% of composite minerals, 0.5 wt% of composite vitamins, and 1 wt% of sunflower oil (the same below) were added to an appropriate amount of water, magnetically stirred at 300 rpm, and sheared at 8000 rpm for 2 min to obtain a vitamin and mineral solution;
[0077] (2) sodium alginate with a final product weight of 1.6 wt%, 1.8 wt%, 2.0 wt%, 2.2 wt%, and 2.4 wt% was uniformly dispersed in water, and fully hydrated under magnetic stirring at 300 rpm for 1-2 h to obtain sodium alginate solutions with different weights;
[0078] (3) Five portions of sodium alginate solution of different masses obtained in step (2) were uniformly dispersed in the vitamin and mineral solution obtained in step (1) to form a gel at 25°C. Subsequently, the solution was sheared at 5000 rpm for 30 seconds to obtain a microgel containing vitamins and minerals. The microgels containing vitamins and minerals obtained in this example were numbered as follows:
[0079] Table 2
[0080]
[0081] Example 3
[0082] A microgel containing vitamins and minerals, the preparation method of which comprises the following steps:
[0083] (1) 0.5 wt% of arabic gum, 0.5 wt% of composite minerals, 0.4 wt% of composite vitamins, and 0.4 wt% of sunflower oil (the same below) were added to an appropriate amount of water, stirred magnetically at 300 rpm, and sheared at 8000 rpm for 2 min to obtain a vitamin and mineral solution;
[0084] (2) 1.6 wt%, 2.0 wt%, 2.4 wt%, 2.8 wt%, and 3.2 wt% of the final product weight of beet pectin were uniformly dispersed in water and fully hydrated under magnetic stirring at 300 rpm for 1-2 h to obtain beet pectin solutions of different weights;
[0085] (3) Five portions of beet pectin solution of different masses obtained in step (2) were uniformly dispersed in the vitamin and mineral solution obtained in step (1), and cross-linked to form a gel at 25°C. Subsequently, microgels containing vitamins and minerals were obtained by shearing at 5000 rpm for 30 seconds. The microgels containing vitamins and minerals obtained in this example were numbered as follows:
[0086] Table 3
[0087]
[0088]
[0089] Example 4
[0090] A microgel containing vitamins and minerals, the preparation method of which comprises the following steps:
[0091] (1) preparing an aqueous solution containing 1 wt% gum arabic, 1 wt% complex minerals, 0.3 wt% complex vitamins, and 0.4 wt% sunflower oil, stirring magnetically at 300 rpm, and shearing at 8000 rpm for 2 min to obtain a vitamin and mineral solution;
[0092] (2) Curdlan powder at 6 wt%, 8 wt%, 10 wt%, 12 wt%, and 14 wt% of the final product weight was directly and evenly dispersed in the vitamin and mineral solution from step (1). The solution was kept at 90°C for 3 min. After cooling, the solution was sheared at 5000 rpm for 30 s to obtain microgels containing vitamins and minerals. The microgels containing vitamins and minerals obtained in this example were numbered as follows:
[0093] Table 4
[0094]
[0095] Example 5
[0096] A microgel containing vitamins and minerals, the preparation method of which comprises the following steps:
[0097] (1) 0.7 wt% of gum arabic, 0.8 wt% of composite minerals, 0.4 wt% of composite vitamins, and 0.6 wt% of sunflower oil were added to an appropriate amount of water, stirred magnetically at 300 rpm, and sheared at 8000 rpm for 2 min to obtain a vitamin and mineral solution;
[0098] (2) low methoxyl pectin with a final product weight of 1.0 wt%, 1.4 wt%, 1.8 wt%, 2.2 wt%, and 2.6 wt% was uniformly dispersed in water, and fully hydrated under magnetic stirring at 300 rpm for 1-2 h to obtain low methoxyl pectin solutions of different weights;
[0099] (3) Five portions of low-methoxyl pectin solution of different masses obtained in step (2) were uniformly dispersed in the vitamin and mineral solution obtained in step (1), and the mixture was kept at 80°C for 2 minutes to form a gel. Subsequently, the mixture was sheared at 5000 rpm for 30 seconds to obtain a microgel containing vitamins and minerals. The microgels containing vitamins and minerals obtained in this example were numbered as follows:
[0100] Table 5
[0101]
[0102] Example 6
[0103] A microgel containing vitamins and minerals, the preparation method of which comprises the following steps:
[0104] (1) 0.8 wt% of gum arabic, 0.7 wt% of composite minerals, 0.4 wt% of composite vitamins, and 0.6 wt% of sunflower oil (the same below) were added to an appropriate amount of water, stirred magnetically at 300 rpm, and sheared at 8000 rpm for 2 min to obtain a vitamin and mineral solution;
[0105] (2) 3.0 wt%, 4.0 wt%, 5.0 wt%, 6.0 wt%, and 7.0 wt% of the final product weight of tamarind gum were uniformly dispersed in water, and fully hydrated under magnetic stirring at 300 rpm for 1-2 h to obtain tamarind gum solutions of different weights;
[0106] (3) Five portions of tamarind gum solution of different masses obtained in step (2) were uniformly dispersed in the vitamin and mineral solution obtained in step (1), and the mixture was kept at 80°C for 2 minutes to form a gel. Subsequently, the mixture was sheared at 5000 rpm for 30 seconds to obtain a microgel containing vitamins and minerals. The microgels containing vitamins and minerals obtained in this example were numbered as follows:
[0107] Table 6
[0108]
[0109]
[0110] Comparative Example 1
[0111] A vitamin and mineral aqueous solution, the preparation method of which comprises the following steps:
[0112] An aqueous solution containing 1.5 wt% of complex minerals and 0.5 wt% of complex vitamins was prepared, and after magnetic stirring at 300 rpm, shearing at 8000 rpm for 2 minutes, a vitamin-mineral aqueous solution was obtained.
[0113] Comparative Example 2
[0114] An aqueous solution containing 0.5 wt% gum arabic, 1.5 wt% complex minerals, 0.5 wt% complex vitamins, 0.5 wt% sunflower oil, and 1.6 wt% amidated low-methoxyl pectin was prepared, and after magnetic stirring at 300 rpm, shearing at 8000 rpm for 2 minutes, a non-gelling vitamin and mineral solution was obtained;
[0115] Performance testing:
[0116] (1) Effect of polysaccharide types on the stability of microgels containing vitamins and minerals:
[0117] The effect of polysaccharide type in the vitamin-mineral microgel formulation on the average particle size, PDI, zeta potential, and viscosity of the microgels was evaluated. Specifically, microgels containing vitamins and minerals were prepared according to the methods described above, including microgel 3 in Example 1, microgel 8 in Example 2, microgel 13 in Example 3, microgel 18 in Example 4, microgel 23 in Example 5, and microgel 28 in Example 6. The average particle size, PDI, zeta potential, and viscosity of microgels 3, 8, 13, 18, 23, and 28 were measured. Table 7 shows the average particle size, PDI, zeta potential, and viscosity of microgels 3, 8, 13, 18, 23, and 28.
[0118] Table 7
[0119]
[0120]
[0121] According to the embodiments, microgel 3, microgel 8, microgel 13, microgel 18, microgel 23, and microgel 28 can all rapidly form stable, uniform gel systems under corresponding gelation conditions. As shown in Table 7, the dispersion coefficients of microgel 3, microgel 8, microgel 13, microgel 18, microgel 23, and microgel 28 are relatively small, essentially presenting a unimodal distribution, with average particle sizes ranging from 350 to 500 nm. All five microgels have a certain amount of surface negative charge, with microgel 3, microgel 8, and microgel 23 exhibiting a relatively large absolute value of zeta potential. The microgels made from microgel 13 and microgel 18 have a relatively high apparent viscosity. In comparison, the viscosities of microgel 3, microgel 8, and microgel 23 are more suitable for direct oral consumption or for administration after rapid dispersion in water.
[0122] (2) Effect of polysaccharide types on the heat resistance and storage stability of microgels containing vitamins and minerals
[0123] The average particle size, PDI, and zeta potential of microgels 3, 8, 13, 18, 23, and 28 were evaluated after heating at 80°C for 20 minutes and storing for 14 days. The average particle size, PDI, and zeta potential were measured using the methods described above. The results are shown in Table 8.
[0124] Table 8
[0125]
[0126]
[0127] After heating and storage, the PDI values of microgels 3, 13, and 23 remained low, while microgels 8, 18, and 28 experienced some particle aggregation and disintegration after storage. The vitamin-mineral microgels prepared with formulations 3, 8, 13, 18, 23, and 28 showed a slight decrease in the absolute value of their zeta potential after simulated pasteurization at 80°C for 20 minutes and storage at room temperature for 14 days. However, they maintained a moderate to strong negative charge overall, demonstrating both heating and storage stability.
[0128] (3) Effects of different polysaccharide addition amounts on the stability of microgels containing vitamins and minerals:
[0129] The average particle size, PDI, zeta potential, and viscosity of vitamin-mineral microgels with varying polysaccharide content were evaluated. Specifically, according to Example 1, the weight of all components except the polysaccharide was kept constant, while the weight of the polysaccharide (amidated low-methoxyl pectin in Example 1 and sodium alginate in Example 2) was varied. The average particle size, PDI, zeta potential, and viscosity were measured using the methods described above. The results are shown in Tables 9 and 10.
[0130] Table 9: Effects of different polysaccharide addition amounts (amidated low methoxyl pectin) on microgels
[0131]
[0132] Table 10: Effects of different polysaccharide additions (sodium alginate) on microgels
[0133]
[0134]
[0135] The strength of gel formation does not increase with increasing polysaccharide content. When the polysaccharide concentration is too low, the system fails to form a gel, manifesting only as an increase in viscosity and a corresponding rise in the absolute value of the zeta potential. When the polysaccharide concentration is too high, the excessively dense negative charge disrupts the system's stable structure, manifesting as a decrease in the absolute value of the zeta potential and a collapse of the particle size, making gel formation and average particle size measurement impossible. Tables 9 and 10 show that when the amidated low-methoxyl pectin concentration is 1.6 wt% or the sodium alginate concentration is 2.0 wt%, the microgels achieve a relatively stable structure with a uniform and narrow particle size distribution.
[0136] (4) Retention of water-soluble vitamins in microgels under different treatment conditions:
[0137] The retention of water-soluble vitamins in the vitamin-mineral microgels of the present invention after heating, storage, and dissolution and subsequent storage was also investigated. Specifically, Comparative Example 1, Comparative Example 2, Microgel 3, and Microgel 8 were prepared. The vitamin C content of these gels and solutions was tested after heating at 80°C for 20 minutes, storing for 14 days, and dissolving in water and then storing for 1 day, respectively. The results are shown in Table 11.
[0138] Table 11: Changes in the content of water-soluble vitamins in microgels after processing in different scenarios
[0139]
[0140] Compared to aqueous vitamin-mineral solutions, microgels 3 and 8 exhibited lower vitamin C loss rates in both simulated pasteurization, 14-day storage, and one-day storage after dilution. In particular, after 14 days of storage, the loss rate decreased by nearly 30%. Compared to Comparative Example 2, this suggests that the microgel structure protects the vitamins, rather than the presence of polysaccharides causing an increase in system viscosity.
[0141] (5) Retention of oil-soluble vitamins in microgels under different treatment conditions:
[0142] Finally, the retention of oil-soluble vitamins in the vitamin-mineral microgels of the present invention after heating, storage, and dissolution was investigated. Specifically, Comparative Example 1, Comparative Example 2, Microgel 3, and Microgel 8 were prepared and tested for their vitamin A, vitamin D, and vitamin E content after heating at 80°C for 20 minutes, storing for 14 days, and dissolving in water and storing for 1 day, respectively. The results are shown in Table 12.
[0143] Table 12: Changes in the content of oil-soluble vitamins in microgels after processing in different scenarios
[0144]
[0145]
[0146] Compared to Comparative Examples 1 and 2, Microgels 3 and 8 demonstrated significantly lower vitamin A, vitamin D, and vitamin E losses in simulated pasteurization and 14-day storage. After 14 days of storage, Microgel 3 reduced vitamin D loss by nearly 60%, while vitamin A and vitamin E losses decreased by nearly 10%. After simulated pasteurization, vitamin D loss decreased by approximately 55%, and vitamin E loss by approximately 40%, demonstrating superior storage and heat resistance. While Microgel 8 was less effective at protecting oil-soluble vitamins than Microgel 3, it also demonstrated improvements in storage and heat resistance compared to the Comparative Examples.
[0147] It can be seen that the microgel containing vitamins and minerals of the present invention has the following advantages:
[0148] (1) The present invention uses the technical concept of microgel to form a gel by mineral induction or heat induction, thereby creating a semi-solid flowable complex vitamin and mineral preparation without the need for additional coagulants, thereby streamlining raw materials and formulas;
[0149] (2) The microgels have a high negative charge (up to -30 mV) and have sufficient electrostatic repulsion to prevent aggregation, so that the minerals can be evenly and stably dispersed in water, and the macroscopic morphology can be maintained stable after long-term storage and heating;
[0150] (3) The microgels of the present invention can simultaneously load water-soluble vitamins and oil-soluble vitamins and possess superior physical stability to vitamin / mineral aqueous solutions. The introduction of polysaccharides acts as a physical barrier between the oil-water interface and the air-water interface, reducing oxidation. Therefore, the microgels of the present invention exhibit superior vitamin retention rates compared to aqueous solutions under heating, storage, and redilution conditions.
[0151] (4) The microgel of the present invention can achieve the loading of a variety of water-soluble vitamins, oil-soluble vitamins and minerals, and has higher nutritional density and function;
[0152] (5) The microgel of the present invention has a softer, viscoelastic texture and good fluidity, and is suitable for meeting the nutritional needs of special groups such as the elderly, infants, patients with dysphagia, and people who exercise.
Claims
1. A high-stability multivitamin mineral microgel carrier, characterized in that: In addition to H2O, the invention also includes the following ingredients by mass: 0.05-1wt% polysaccharide 1, 1.2-14wt% polysaccharide 2, 0.5-1.5wt% complex minerals, 0.3-0.5wt% complex vitamins, and 0.4-1wt% liquid oil; the polysaccharide 1 is one or more of sodium carboxymethyl cellulose, sodium methyl cellulose, gum arabic, soybean polysaccharide, pectin, citrus fiber, chitosan, and xanthan gum; the polysaccharide 2 is one or more of low-methoxyl pectin, amidated low-methoxyl pectin, beet pectin, curdlan, tamarind gum, and sodium alginate; and the complex minerals are one or more of inorganic salts and / or organic salts of sodium, potassium, copper, magnesium, iron, zinc, manganese, calcium, phosphorus, iodine, chlorine, and selenium.
2. A high-stability multivitamin mineral microgel carrier according to claim 1, characterized in that: The complex vitamins are one or more of water-soluble vitamins and oil-soluble vitamins.
3. A high-stability multivitamin mineral microgel carrier according to claim 2, characterized in that: The water-soluble vitamins are one or more of vitamin B1, vitamin B2, vitamin B6, vitamin B12, niacin, folic acid, pantothenic acid, vitamin C and biotin.
4. The vitamin / mineral-containing microgel according to claim 2, characterized in that The oil-soluble vitamins are one or more of vitamin A, vitamin D, vitamin E, and vitamin K1.
5. The vitamin / mineral-containing microgel according to claim 1, characterized in that The liquid oil is one or more of sunflower oil, corn oil, soybean oil, rapeseed oil, peanut oil, olive oil, fish oil, algae oil, perilla oil, linseed oil, chia seed oil, medium chain triglycerides, and diglycerides.
6. The method for preparing the high-stability multivitamin mineral microgel carrier according to any one of claims 1 to 5, characterized in that The following steps are involved: Step 1. Preparation of vitamin / mineral emulsion: shearing multivitamins, multiminerals, liquid oil, polysaccharide 1 and an appropriate amount of water to obtain a vitamin / mineral emulsion; Step 2. Preparation of polysaccharide 2 aqueous solution: dissolving polysaccharide 2 in an appropriate amount of water with stirring to obtain a fully hydrated polysaccharide 2 solution; Step 3. Microgel formation: The polysaccharide 2 aqueous solution is mixed with the vitamin / mineral emulsion, kept at a set temperature, and then sheared to form a microgel.
7. The preparation method according to claim 6, characterized in that The shear rate in step 1 is 5000-10000 rpm, and the shear time is 1-2 min.
8. The preparation method according to claim 6, characterized in that The insulation temperature in step 3 is 20-90° C., and the insulation time is 2-5 minutes.
9. The preparation method according to claim 5, characterized in that The shear rate in step 3 is 3000-6000 rpm, and the shear time is 0.5-1 min.
10. Use of the high-stability multivitamin mineral microgel carrier according to claim 1 in food and beverages, RTD nutritional health products, sports nutrition foods or liquid special medical foods.
Citation Information
Patent Citations
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