Embedding method for stabilizing and slowly releasing beta-carotene

Abstract

The invention discloses an embedding method for stabilizing and slowly releasing beta-carotene. The embedding method comprises the following steps: selecting soybean oil; the stirring conditions are as follows: 300 r / min and 75 DEG C; preparing a water phase: stirring 80 kg of maltodextrin and 20 kg of cane sugar at 50 DEG C until 200 kg of distilled water is completely dissolved; the homogenizing conditions are as follows: the high-speed mixing and shearing emulsifying machine shears for 5 minutes at the speed of 17000 r / min, and the high-pressure homogenizing machine homogenizes for 2 minutes at the pressure of 20 MPa; the spray drying conditions are as follows: the pressure is 0.5 MPa, the inlet temperature is 170 DEG C, and the flow rate is 10 mL / min. The particle size D of the optimized beta-carotene microcapsule product is 95lt; according to the present invention, the prepared nano-particles have characteristics of uniform particle size, 300 nm, embedding rate of 94.2%, good stability in the 90-day storage period, and significantly improved solubility.

Description

TECHNICAL FIELD

[0001] The present application relates to the field of food engineering and biotechnology, in particular to an embedding technology for improving the stability and prolonging the slow-release effect of β-carotene, which is especially suitable for the preparation of β-carotene microcapsule products in the food, pharmaceutical and cosmetic industries. BACKGROUND

[0002] Carotenoids are widely present in nature and are an important class of natural pigments with strong antioxidant capacity and significant physiological activity. Current commercial carotenoid products mainly include β-carotene, astaxanthin, lycopene, canthaxanthin and lutein, etc. These carotenoids have been widely used in food, cosmetics, feed and medicine as nutritional fortifiers and natural colorants. Among them, β-carotene, as a precursor of vitamin A, plays an important role in promoting visual health, enhancing immunity, and resisting oxidation and aging. Therefore, the development of efficient and stable β-carotene preparations has important commercial value and social significance.

[0003] However, β-carotene has strong hydrophobicity and very low solubility in water, and its solubility in oil is also poor. Due to the presence of a large number of unsaturated carbon-carbon double bonds in its structure, β-carotene is extremely sensitive to oxidation, heat and light, and is easily degraded and deteriorated during storage. When β-carotene exists in the form of coarse crystals, its particles are large, the taste is poor, and the absorption and utilization rate in the human body is low, which seriously affects its application effect in food, medicine and cosmetics.

[0004] In order to improve the solubility and stability of β-carotene and improve its dispersion performance in aqueous medium, various embedding and microencapsulation preparation methods have been developed in the prior art. At present, the preparation process of β-carotene embedding preparation mainly includes grinding method, organic solvent method, solvent replacement method, spray drying method, freeze drying method and nano-emulsion method, etc.

[0005] Patents WO91 / 06292 and WO94 / 19411 introduce a method of using a colloid mill to grind β-carotene into microparticles of 2-10 μm, and then drying to prepare a water-dispersible carotenoid powder. Although this method is relatively simple, the grinding method has low efficiency and high energy consumption, and the particle size of β-carotene is large, which is difficult to further reduce to below 1 μm, resulting in poor bioavailability.

[0006] US Patent 3998753 discloses a method for preparing water-dispersible β-carotene. This method involves mixing β-carotene with gelatin, dispersants, stabilizers, and other components, dissolving it in an organic solvent, and then adding the mixture to an aqueous phase. The mixture is then emulsified under high-speed shearing to form an emulsion. The organic solvent is removed, and the mixture is spray-dried to form microcapsule powder. This method can significantly improve the dispersibility and stability of β-carotene, but it suffers from the problem of residual organic solvent. Due to the limited solubility of β-carotene in organic solvents, this method still struggles to achieve the preparation of stable microcapsules with high β-carotene content.

[0007] US Patent 4522743 discloses a method for dissolving β-carotene in a volatile water-miscible solvent at 50–200°C, then rapidly mixing it with an aqueous solution containing a protective colloid, and finally mixing at 0–50°C to form an emulsion. This method can obtain β-carotene microparticles with a particle size of less than 0.5 μm in a relatively short time. However, this method requires operation under high pressure (3.0–6.0 MPa) and high temperature (170–200°C), which places high demands on equipment, poses certain safety hazards, and makes the operation process control relatively complex, thus making industrial application difficult.

[0008] Patent CN1836652A describes a dual-solvent method for preparing β-carotene microcapsules. This method uses antioxidants and emulsifiers to dissolve crude β-carotene crystals in a halogenated hydrocarbon or ester solvent. The resulting solution is then sprayed into rapidly stirred ethanol or isopropanol, precipitating carotenoid powder. The powder is subsequently filtered through a membrane, washed, and dried to obtain the carotenoid microcapsule formulation. While this method effectively reduces residual organic solvents and significantly improves the stability of carotenoids, the resulting product suffers from a β-carotene loss rate as high as 40%, and the β-carotene crystals remain relatively large, affecting their absorption and utilization.

[0009] Patent CN101016259A, based on the aforementioned dual-solvent method, further increases the content of the all-trans isomer in β-carotene formulations by adding a combination of antioxidants. Although this method has some effect on improving the stability of β-carotene, the crystal size of β-carotene in the product is still 0.7–0.9 μm, and the bioavailability remains insufficient.

[0010] US2005 / 0037115 discloses a method for dissolving β-carotene in fatty acid esters, adding the resulting solution to an aqueous phase containing a dispersant, and then evaporating the solvent to obtain a nanoscale dispersion. Although this method effectively reduces the crystal size of β-carotene, the extremely low solubility of β-carotene in fatty acid esters results in a low β-carotene content in the final product, limiting its industrial application.

[0011] In summary, existing β-carotene encapsulation technologies generally suffer from the following problems: 1) Many methods rely on organic solvents, which can lead to solvent residue problems and potentially have adverse effects on health and safety.

[0012] 2) Some methods and processes are complex and require advanced equipment, which is not conducive to large-scale industrial production.

[0013] 3) Existing methods have certain shortcomings in improving the reduction of β-carotene crystal size and the stability of the all-trans isomer, which affects its bioavailability and product quality.

[0014] To address the shortcomings of existing technologies, this invention proposes an improved β-carotene encapsulation method. This method significantly improves the encapsulation rate and stability of β-carotene by optimizing the oil-water phase ratio, improving homogenization, and spray drying processes. This invention uses maltodextrin, sucrose, and SE-11 sucrose fatty acid emulsifier as wall materials, combined with oil-phase emulsification conditions of 300 r / min, 75℃, and 3 h of stirring, and optimized parameters of 17000 r / min shearing for 5 min and high-pressure homogenization at 20 MPa for 2 min to ensure the homogeneity and stability of the emulsion. Finally, microcapsule powder is prepared by spray drying at 0.5 MPa pressure, 170℃ inlet temperature, and 10 mL / min feed flow rate, significantly improving the β-carotene encapsulation rate (≥94%) and retention rate (≥93% after 90 days of storage).

[0015] The β-carotene encapsulation method provided by this invention has the advantages of simple operation, stable process, low energy consumption, and environmental friendliness. It can effectively improve the stability and bioavailability of β-carotene and has high value for industrial application. Summary of the Invention

[0016] The purpose of this invention is to overcome the defects of existing technologies, such as poor stability, rapid oxidative degradation, and poor product dispersibility and solubility of β-carotene during encapsulation, and to provide a method for preparing nanoscale β-carotene microcapsules that can significantly improve the stability of β-carotene and have excellent dispersibility and solubility.

[0017] This invention discloses an encapsulation method for stabilizing and sustaining the release of β-carotene, characterized by the following steps: 1) Preparation of β-carotene oil phase solution: β-carotene is added to vegetable oil and stirred at 300 r / min for 3 hours at 75℃. During the stirring process, a uniform oil phase solution is gradually formed to ensure that β-carotene is fully dissolved and uniformly dispersed, thereby reducing its risk of oxidative degradation. The edible oils mentioned are: soybean oil, corn oil, and olive oil, and the mass ratio of vegetable oil to β-carotene is 1-2:1. 2) Preparation of aqueous solution: Add maltodextrin, sucrose and distilled water to an emulsifying tank, and stir at 40-60℃ for 30-60 minutes until completely dissolved. Stir until the solution is transparent, without bubbles or foam. The mass ratio of maltodextrin to sucrose is 3-6:1. 3) Homogenization and emulsification: Slowly pour the oil phase solution obtained in step 1) into the aqueous phase solution obtained in step 2), and add 1.5 kg of SE-11 sucrose fatty acid as an emulsifier; use a high-speed mixing shear emulsifier at 17000 r / min and 25℃ for 5-15 minutes to fully emulsify the oil phase into an oil-in-water (O / W) type primary emulsion; then, transfer the emulsion to a high-pressure homogenizer and homogenize it at 10-30 MPa for 1-3 minutes to further refine and uniformly disperse the emulsion, obtaining a β-carotene emulsion with a smaller particle size; the emulsion is then allowed to stand for 12 hours to further stabilize the emulsion structure.

[0018] 4) Spray drying: The emulsion is dried using a spray dryer. The spray drying parameters are: atomization pressure 3-8 MPa, inlet temperature 150-200℃, and feed flow rate 5-15 mL / min. Appropriate temperature and atomization conditions are controlled during the drying process to avoid thermal degradation of β-carotene. The resulting β-carotene microcapsules exhibit good nanoscale dispersibility and high stability. Among them: Step 1) The mass ratio of vegetable oil to β-carotene is 1.5:1; the vegetable oil is soybean oil.

[0019] Step 2) The mass ratio of maltodextrin to sucrose is 4:1; the dissolution temperature is 50-55℃; and the dissolution time is 40 minutes.

[0020] In step 3), the high-speed shearing time is 8-10 minutes; the homogenization pressure is 20 MPa; and the homogenization is performed twice.

[0021] In step 4), the spray drying conditions are: atomization pressure of 0.5 MPa; inlet temperature of 170℃; and feed rate of 10 mL / min.

[0022] This invention further discloses the application of β-carotene prepared using an improved β-carotene encapsulation method in improving the particle size and storage stability of β-carotene microcapsule products. Experimental results show that the optimized β-carotene microcapsule product has a particle size D95 < 300 nm, an encapsulation rate of 94.2%, maintains good stability during a 90-day storage period, and exhibits significantly improved solubility.

[0023] The core of this invention lies in optimizing the oil and water phase formulations, controlling homogenization and spray drying conditions, so that the β-carotene crystal particle size reaches the nanoscale (D95<300 nm), which significantly improves the product's stability, solubility and bioavailability.

[0024] The encapsulation method for stabilizing and sustaining the release of β-carotene disclosed in this invention has the following advantages compared with the prior art: Using vegetable oil as the oil phase matrix optimizes the use of soybean oil, further reducing the risk of oxidative degradation of β-carotene due to temperature increases during grinding and emulsification. Wall material optimization: maltodextrin and sucrose are used as wall materials, significantly improving the encapsulation efficiency and stability of the microcapsules. Homogenization and emulsification optimization: High-speed shearing and high-pressure homogenization processes allow for nanoscale control of β-carotene particle size, improving its bioavailability and stability. Spray drying optimization: Optimized spray drying process conditions significantly improve the dispersibility, solubility, and storage stability of the microcapsules. Solvent-free process: This method avoids the use of organic solvents, making it safer and more environmentally friendly, while also reducing production costs. Nanoscale particles: The final β-carotene microcapsule product has a D95 < 300 nm, significantly improving stability, solubility, and bioavailability, meeting the application needs of food, health products, and other fields. Detailed Implementation

[0025] The present invention will now be described through specific embodiments. Unless otherwise specified, all technical means used in this invention are methods well known to those skilled in the art. Furthermore, the embodiments should be understood as illustrative, not limiting the scope of the invention; the essence and scope of the invention are defined only by the claims. For those skilled in the art, various changes or modifications to the material composition and dosage in these embodiments without departing from the essence and scope of the invention are also within the scope of protection of this invention. All raw materials and reagents used in this invention are commercially available.

[0026] I. Main raw material sources for the example: β-carotene (purity ≥98%); soybean oil (food grade); maltodextrin (DE value 10-20) Sucrose (food grade); SE-11 sucrose fatty acid (emulsifier); other reagents are all general commercially available chemically pure reagents.

[0027] II. Main analytical methods and instruments: Ball mill: Model XX-200; High-speed shear mill: Model SRH-17000; High-pressure homogenizer: Model JNG-20 Spray dryer: Model SD-5MPA; Emulsification tank: equipped with a stirrer and temperature control system. Example

[0028] 1) Preparation of β-carotene oil phase solution: 10 kg of β-carotene was added to 20 kg of soybean oil, and stirred at 300 r / min and 75℃ for 3 h until a stable and homogeneous oil phase solution was formed. The oil phase solution exhibited good fluidity during emulsification, ensuring thorough dispersion of β-carotene and significantly reducing the risk of oxidative degradation.

[0029] 2) Preparation of the aqueous solution: Add 80 kg of maltodextrin, 20 kg of sucrose, and 200 kg of distilled water to an emulsifying tank. Maintain the stirring temperature at 50°C and continue stirring until completely dissolved. The optimized aqueous solution should be transparent, free of bubbles and floating matter, to ensure the homogeneity and stability of the aqueous phase.

[0030] 3) Homogenization and Emulsification: The oil and aqueous phases were mixed, and 1.5 kg of SE-11 sucrose fatty acid emulsifier was added. A high-speed mixing shear emulsifier was used at 17000 r / min and 25℃ for 5 min to initially emulsify into an oil-in-water (O / W) type primary emulsion. The primary emulsion was then transferred to a high-pressure homogenizer, with the pressure controlled at 20 MPa and homogenization time at 2 min to further refine the emulsion particles. After completion, the emulsion was allowed to stand for 12 h to enhance stability.

[0031] 4) Spray drying: The emulsion after standing was transferred to a spray dryer with the following parameters set: spray dryer pressure: 0.5 MPa, inlet temperature: 170℃, flow rate: 10 mL / min; The resulting β-carotene microcapsules were a light yellow powder with a particle size D95 < 300 nm, exhibiting good flowability, solubility, and stability.

[0032] Comparative Example 1 Optimization experiment of oil phase solution In the preparation of β-carotene oil phase solutions, three different vegetable oils were selected as oil phase matrices: soybean oil, corn oil, and olive oil. In the experiment, equal amounts of β-carotene powder (10 kg) were added to 20 kg of soybean oil, corn oil, and olive oil, respectively. The stirring rate was controlled at 300 r / min, the temperature at 75℃, and stirring was continued for 3 h. After stirring, the homogeneity and stability of each group of oil phase solutions were observed, and the solutions were sealed and stored at 25℃ for 90 days. During this period, the β-carotene content of the solutions was measured periodically to assess their stability.

[0033] The comparison results of data from Example 1 and Comparative Example 1 are shown in Table 1.

[0034] Experimental results showed that soybean oil exhibited good solubility, optimal stability, and the highest encapsulation rate of β-carotene. Therefore, soybean oil was ultimately selected as the oil phase matrix.

[0035] Comparative Example 2 Experiment on optimization of stirring parameters In the preparation of oil phase solutions, different stirring rates and times affect the stability of the solution.

[0036] In the experiment, equal amounts of a mixture of β-carotene and soybean oil were used, and the stirring rates were set to 300 r / min and 400 r / min, respectively, for 2 h and 3 h. After stirring, the resulting oil phase solution was sealed and stored, and its appearance and color changes were observed periodically, and the degradation rate of β-carotene was tested.

[0037] The comparison results of data from Example 1 and Comparative Example 2 are shown in Table 2.

[0038]

[0039] The results showed that the oil phase solution was most stable and the degradation rate of β-carotene was lowest when the stirring rate was 300 r / min and the stirring time was 3 h. Therefore, this condition was selected as the optimal stirring parameters.

[0040] Comparative Example 3 Optimization experiment of aqueous solution The stability of the aqueous solution plays a crucial role in the quality of the final emulsion.

[0041] In the experiment, maltodextrin (80 kg and 60 kg) and sucrose (10 kg and 20 kg) were added to 200 kg of distilled water in different proportions. The stirring temperatures were set at 50℃ and 55℃, respectively, and the mixture was stirred until the raw materials were completely dissolved. The appearance, bubble formation, and precipitation of the aqueous solution were then observed, and the solution was stored for 60 days to test its long-term stability.

[0042] The results of comparing the data of Example 1 and Comparative Example 3 are shown in Table 3.

[0043]

[0044] The results showed that when the amount of maltodextrin was 80 kg, the amount of sucrose was 20 kg, and the stirring temperature was controlled at 50℃, the resulting aqueous solution was the clearest, most transparent, foam-free, and precipitate-free, and also exhibited the best long-term stability. Therefore, this formulation and conditions were determined to be the optimal aqueous solution preparation process.

[0045] Comparative Example 4 Optimization experiment of homogeneous parameters The homogenization process plays a crucial role in the particle size distribution and stability of emulsions.

[0046] In the experiment, the oil and aqueous phases were mixed in the aforementioned proportions, and 1.5 kg of SE-11 sucrose fatty acids were added as an emulsifier. A high-speed mixing shear emulsifier was used, and shearing was performed at speeds of 15000 r / min, 17000 r / min, and 20000 r / min for 3 min or 5 min, respectively. After shearing, a high-pressure homogenizer was used, with pressures set at 15 MPa and 20 MPa, and homogenization times of 1 min and 2 min, respectively.

[0047] The results of comparing the data of Example 1 and Comparative Example 4 are shown in Table 4.

[0048]

[0049] Experimental results show that the emulsion with the smallest particle size (D95 approximately 3.8 μm) obtained by using a high-speed mixing shear emulsifier with stirring at 17000 r / min for 5 min and a high-pressure homogenizer with homogenization at 20 MPa for 2 min exhibits better dispersion and stability. Therefore, this parameter combination was determined to be the optimal homogenization condition.

[0050] Comparative Example 5 Optimization experiment of spray drying parameters Spray drying parameters have a significant impact on the appearance, particle size, and flowability of β-carotene microcapsules.

[0051] In the experiment, the same volume of emulsion was taken, and the spray dryer pressure was set to 0.4 MPa, 0.5 MPa and 0.6 MPa respectively; the inlet temperature was set to 160℃, 170℃ and 180℃ respectively; and the flow rate was set to 8 mL / min, 10 mL / min and 12 mL / min respectively.

[0052] The comparison results of data from Example 1 and Comparative Example 5 are shown in Table 5.

[0053]

[0054]

[0055] Experimental results show that when the spray drying pressure is 0.5 MPa, the inlet temperature is 170℃, and the flow rate is 10 mL / min, the particle size D95 of the obtained β-carotene microcapsules is less than 300 nm, the powder is light yellow, has good flowability and solubility, and has the best storage stability.

[0056] Summary of Optimization Experiments: Through the above series of optimization experiments, the optimal process parameters were finally determined as follows: Oil phase matrix: soybean oil was used; stirring conditions: 300 r / min, 75℃ for 3 h; aqueous phase preparation: 80 kg maltodextrin, 20 kg sucrose, stirred at 50℃ until completely dissolved in 200 kg distilled water; homogenization conditions: high-speed mixing shear emulsifier at 17000 r / min for 5 min, high-pressure homogenizer at 20 MPa for 2 min; spray drying conditions: pressure 0.5 MPa, inlet temperature 170℃, flow rate 10 mL / min.

[0057]

[0058] Conclusion: This invention proposes an improved method for encapsulating β-carotene. By optimizing the oil-to-water phase ratio and improving homogenization and spray drying processes, this method significantly improves the encapsulation efficiency, stability, and bioavailability of β-carotene. This encapsulation method is simple to operate, has stable processes, low energy consumption, and is environmentally friendly, making it highly valuable for industrial application.

Claims

1. An encapsulation method for stabilizing and sustaining the release of β-carotene, characterized in that... Follow these steps: 1) Preparation of β-carotene oil phase solution: β-carotene is added to vegetable oil and stirred at 300 r / min for 3 hours at 75℃. During the stirring process, a uniform oil phase solution is gradually formed. The edible oil refers to peanut oil, flaxseed oil, and sunflower seed oil. The mass ratio of vegetable oil to β-carotene is 1-2:

1. 2) Preparation of aqueous solution: Add maltodextrin, sucrose and distilled water to an emulsifying tank, and stir at 40-60℃ for 30-60 minutes until completely dissolved. Stir until the solution is transparent, without bubbles or foam. The mass ratio of maltodextrin to sucrose is 3-6:

1. 3) Homogenization and emulsification: Slowly pour the oil phase solution obtained in step 1) into the aqueous phase solution obtained in step 2), while adding 1.5 kg of SE-11 sucrose fatty acid as an emulsifier; use a high-speed mixing shear emulsifier at 17000 r / min and 25℃ for 5-15 minutes to fully emulsify the oil phase into an oil-in-water (O / W) type primary emulsion; then, transfer the emulsion to a high-pressure homogenizer and homogenize it at 10-30 MPa for 1-3 minutes to further refine and uniformly disperse the emulsion, obtaining a β-carotene emulsion with a smaller particle size; the emulsion is then allowed to stand for 12 hours; 4) Spray drying: The emulsion is dried by a spray dryer. The spray drying parameters are: atomization pressure 3-8 MPa, inlet temperature 150-200℃, and feed flow rate 5-15 mL / min.

2. The encapsulation method for stabilizing and sustaining the release of β-carotene according to claim 1, characterized in that... Step 1) The mass ratio of vegetable oil to β-carotene is 1.5:1; the vegetable oil is soybean oil.

3. The encapsulation method for stabilizing and sustaining the release of β-carotene according to claim 1, characterized in that... Step 2) The mass ratio of maltodextrin to sucrose is 4:1; the dissolution temperature is 50-55℃; and the dissolution time is 40 minutes.

4. The encapsulation method for stabilizing and sustaining the release of β-carotene according to claim 1, characterized in that... In step 3), the high-speed shearing time is 8-10 minutes; the homogenization pressure is 20 MPa; and the homogenization is performed twice.

5. The encapsulation method for stabilizing and sustaining the release of β-carotene according to claim 1, characterized in that... In step 4), the spray drying conditions are: atomization pressure of 0.5 MPa; inlet temperature of 170℃; and feed rate of 10 mL / min.

6. The β-carotene prepared by the method described in claim 1 can be controlled at the nanoscale, which significantly improves its stability, solubility and bioavailability. The β-carotene encapsulation method provided has the advantages of simple operation, stable process, low energy consumption and environmental friendliness, which meets the application needs of food, health products and other fields.

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