Preparation method of carotenoid
Through microcapsule technology, carotenoid microcapsules are prepared using raw materials such as lignin sulfonate, which solves the problem of poor hygroscopicity and stability of existing carotenoid preparations, achieves higher anti-hygroscopic properties and stability, and improves the quality and bioavailability of the product.
Patent Information
- Application Number
- CN202411937905.1
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2024-12-26
- Publication Date
- 2025-04-11
AI Technical Summary
The existing carotenoid preparations have problems of poor hygroscopicity and stability, which leads to their easy absorption of water and changes in physical properties in humid environments, and their long-term storage stability is poor.
Using microcapsule technology, carotenoids are mixed with raw materials such as lignin sulfonates, fillers, crosslinking agents and antioxidants in a specific proportion, and microcapsules are prepared by spray drying to form a dense protective layer to improve anti-hygroscopic properties and stability.
It significantly improves the anti-hygroscopic properties and stability of microcapsules, extends storage time, and improves product quality and bioavailability.
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Abstract
Description
Technical Field
[0001] The invention relates to the field of microcapsule pigment preparations, and solves the problems of poor hygroscopicity, poor stability, low bioavailability and the like of existing products. Background Art
[0002] Carotenoids are a class of organic pigments that are widely found in nature, ranging in color from bright yellow to deep red. These pigments are produced naturally by a variety of biological organisms, including photosynthetic organisms such as plants, algae and certain bacteria (e.g., cyanobacteria), as well as some fungi. In nature, carotenoids play a vital role. Not only do they give carrots their signature orange color, they also provide flamingos and salmon with an attractive pink color, and give lobsters and shrimp their attractive red color.
[0003] It is important to note that, despite the ubiquity of carotenoids in nature, animals are unable to synthesize these pigments themselves, so they must obtain them through their diet. In the industrial sector, carotenoids are widely used in the food and feed industries. Not only do they provide rich colors to products, they also have important nutritional functions and enhance consumer acceptance. For example, astaxanthin is a common carotenoid that is widely used in salmon aquaculture to ensure that farmed salmon have similar pink or red pigmentation characteristics to wild salmon.
[0004] In addition, some carotenoids have potential health benefits. For example, some carotenoids can serve as precursors to vitamin A, helping to maintain normal vision and immune function. At the same time, they also have antioxidant properties that can help protect cells from damage by free radicals, thereby potentially reducing the risk of certain chronic diseases. Currently, some carotenoids such as beta-carotene, lycopene, astaxanthin, zeaxanthin and lutein have been developed into nutritional supplements for people to supplement these beneficial pigments in their daily diet. These supplements are popular in the market because they can help people gain more health benefits while also adding attractive colors to food.
[0005] Carotenoid preparations prepared using lignin sulfonate as the main ingredient have some significant problems, especially poor performance in terms of hygroscopicity and storage stability. Specifically, this type of preparation easily absorbs moisture in a humid environment, causing changes in its physical properties, thereby affecting its use effect and quality. In addition, due to the chemical structure and properties of lignin sulfonate, carotenoid preparations have poor stability during long-term storage and are prone to decomposition or deterioration, further limiting their scope of application and market prospects. The existence of these problems requires researchers and manufacturers to find new solutions to improve the hygroscopicity and storage stability of carotenoid preparations in order to meet market demand and improve product quality. Summary of the invention
[0006] The purpose of the present invention is to provide a microcapsule pigment preparation to solve the problems of poor hygroscopicity, stability and low bioavailability of existing products.
[0007] To achieve the object of the present invention, the present invention provides a carotenoid microcapsule preparation, which is prepared from the following raw materials in parts by weight:
[0008] 5-20 parts of carotenoids, 40-80 parts of lignin sulfonate, 2-20 parts of fillers, 2-10 parts of cross-linking agents, 2-5 parts of antioxidants, and 60-160 parts of water.
[0009] In the present invention, the lignin sulfonate is sodium lignin sulfonate or calcium lignin sulfonate, with a molecular weight of 800-100000 and a sulfonation degree of 40-70%.
[0010] In the present invention, the filler is at least one selected from sucrose, maltose, glucose and syrup.
[0011] In the present invention, the cross-linking agent is selected from at least one of xanthan gum, carboxymethyl cellulose, methyl cellulose, polymaleic acid and succinic acid.
[0012] In the present invention, the antioxidant is selected from at least one of tocopherol, fatty acid ascorbic acid ester, butylated hydroxytoluene (BHT), butylated hydroxyanisole (BHA), propyl gallic acid, and tert-butylhydroxyquinoline.
[0013] On the other hand, the present invention also provides a method for preparing carotenoid microcapsules, the method comprising the following steps:
[0014] 1) dissolving lignin sulfonate in water, heating, stirring until uniformly dispersed, and adding filler to form aqueous phase a);
[0015] 2) mixing the carotenoids and the antioxidant to obtain an oil phase b);
[0016] 3) adding the oil phase b) into the water phase a), mixing, shearing and stirring to obtain a mixed phase c);
[0017] 4) adding a crosslinking agent to the mixed phase c) in step 3), heating and stirring to obtain an emulsion d);
[0018] 5) spray drying the emulsion d) obtained in step 4) to obtain carotenoid microcapsules.
[0019] In the present invention, the heating temperature in step 1) is 60-65° C., the stirring speed is 2000-4000 rpm, and the stirring time is 10-120 min;
[0020] In the present invention, the shearing speed in step 3) is 6000-7000 rpm, and the shearing time is 10-90 min;
[0021] In the present invention, the heating temperature in step 4) is 80°C to 190°C; the cross-linking time is 15 to 24 hours;
[0022] In the present invention, in step 5), the spray drying temperature is 80-85° C., and the atomizer speed is 30-35 Hz.
[0023] The beneficial effects of the present invention are:
[0024] 1. Compared with the existing technology, the present invention can effectively promote the formation of intermolecular hydrogen bonds between lignin sulfonate molecules through cross-linking reaction. The mutual attraction of these intermolecular hydrogen bonds enables a dense protective layer to be formed on the surface of lignin sulfonate. This structure not only gives the microcapsule excellent anti-hygroscopic performance, but also significantly improves its stability, thereby greatly improving the stability during storage.
[0025] 2. In addition, the present invention uses lignin sulfonate as the wall material of the microcapsule, which not only significantly reduces the production cost, but also has many other advantages. First, lignin sulfonate as a wall material has excellent degradation performance and can be decomposed by microorganisms in the natural environment within a short time after use, thereby reducing the risk of environmental pollution. Secondly, lignin sulfonate has good environmental compatibility and will not cause new pollution sources to the environment such as water bodies, air and soil. Therefore, the present invention not only has significant advantages in economic benefits, but also performs well in environmental protection, providing a new idea for the sustainable development of microcapsule technology. DETAILED DESCRIPTION
[0026] The sources of the raw materials or reagents used in the examples and comparative examples of the present invention are as follows, and the others are all commercially available products unless otherwise specified:
[0027] Carotenoid crystals were purchased from Chenguang Biotechnology;
[0028] Calcium lignin sulfonate with a molecular weight of 800 and sodium lignin sulfonate with a molecular weight of 1000 were purchased from Wuhan Xinyingda Chemical Co., Ltd. and Shenyang Xingzhenghe Chemical Co., Ltd.;
[0029] The test methods used in the embodiments and comparative examples of the present invention are as follows. Unless otherwise specified, other test equipment and test methods are conventional in the art:
[0030] (1) Viscosity: viscometer BROOK CAP2000;
[0031] (2) Average particle size: Malvern laser particle size analyzer Mastersizer 3000;
[0032] (3) Content of all-trans isomer: High performance liquid chromatography, analysis conditions: Agilent liquid chromatography polysiloxane column HP-5 was used for determination, two-step temperature program, initial temperature 120°C, maintained for 1 minute, then increased to 100°C at a rate of 10°C / min, and then increased to 250°C at a rate of 15°C / min; carrier gas was high-purity N2, split ratio 150:1; injection temperature was 250°C, detector was FID, detector temperature was 260°C; injection volume was 0.5 μL.
[0033] Example 1
[0034] 1) 40 g of sodium lignin sulfonate, wherein the degree of sulfonation is 40%, is dissolved in 60 g of water, heated to 60° C., stirred at 2000 rpm until uniformly dispersed, and then 2 g of glucose as a filler is added to form an aqueous phase a);
[0035] 2) mixing 5 g of carotenoids with 2 g of antioxidant BHT to obtain an oil phase b);
[0036] 3) adding the oil phase b) into the water phase a), mixing, stirring at a shearing speed of 6000prm, to obtain a mixed phase c);
[0037] 4) adding 2 g of xanthan gum as a crosslinking agent (directly added) to the mixed phase c) in step 3), heating at 80° C. for 15 h, and stirring to obtain an emulsion d);
[0038] 5) spray drying the emulsion d) obtained in step 4) at a spray drying temperature of 80° C. and an atomizer speed of 30 Hz to obtain carotenoid microcapsules with a carotene particle size D50 of 207 μm and a carotene content of 9.6%.
[0039] Example 2
[0040] 1) 80 g of calcium lignin sulfonate, wherein the degree of sulfonation is 70%, is dissolved in 160 g of water, heated to 65° C., stirred at 4000 rpm until uniformly dispersed, and then 20 g of filler sucrose is added to form an aqueous phase a);
[0041] 2) mixing 20 g of carotenoids with 5 g of antioxidant BHT to obtain an oil phase b);
[0042] 3) adding the oil phase b) into the water phase a), mixing, stirring at a shearing speed of 7000prm, to obtain a mixed phase c);
[0043] 4) adding 10 g of xanthan gum (directly added) as a crosslinking agent to the mixed phase c) in step 3), heating at 150° C. for 20 h, and stirring to obtain an emulsion d);
[0044] 5) spray drying the emulsion d) obtained in step 4) at a spray drying temperature of 85° C. and an atomizer speed of 35 Hz to obtain carotenoid microcapsules with a carotene particle size D50 of 204 μm and a carotene content of 3.67%.
[0045] Example 3
[0046] 1) 60 g of sodium lignin sulfonate, wherein the degree of sulfonation is 60%, is dissolved in 80 g of water, heated to 62° C., stirred at 3000 rpm until uniformly dispersed, and 10 g of maltose as a filler is added to form an aqueous phase a);
[0047] 2) mixing 10 g of carotenoids with 3 g of antioxidant BHA to obtain an oil phase b);
[0048] 3) adding the oil phase b) into the water phase a), mixing, stirring at a shearing speed of 6500prm, to obtain a mixed phase c);
[0049] 4) adding 7 g of methyl cellulose as a crosslinking agent (directly) to the mixed phase c) in step 3), heating at 100° C. for 24 h, and stirring to obtain an emulsion d);
[0050] 5) spray drying the emulsion d) obtained in step 4) at a spray drying temperature of 83° C. and an atomizer speed of 33 Hz to obtain carotenoid microcapsules with a carotene particle size D50 of 310 μm and a carotene content of 5.50%.
[0051] Example 4
[0052] 1) 60 g of sodium lignin sulfonate, wherein the degree of sulfonation is 40%, is dissolved in 60 g of water, heated to 60° C., stirred at 2500 rpm until uniformly dispersed, and then 2 g of filler syrup is added to form an aqueous phase a);
[0053] 2) mixing 10 g of carotenoids with 2 g of antioxidant tert-butylhydroxyquinoline to obtain an oil phase b);
[0054] 3) adding the oil phase b) into the water phase a), mixing, stirring at a shearing speed of 6000prm, to obtain a mixed phase c);
[0055] 4) adding 2 g of succinic acid as a crosslinking agent (directly) to the mixed phase c) in step 3), heating at 80° C. for 15 h, and stirring to obtain an emulsion d);
[0056] 5) spray drying the emulsion d) obtained in step 4) at a spray drying temperature of 80° C. and an atomizer speed of 30 Hz to obtain carotenoid microcapsules with a carotene particle size D50 of 300 μm and a carotene content of 7.02%.
[0057] Example 5
[0058] 1) 40 g of calcium lignin sulfonate, wherein the degree of sulfonation is 50%, is dissolved in 100 g of water, heated to 64° C., stirred at 3200 rpm until uniformly dispersed, and 15 g of filler glucose is added to form an aqueous phase a);
[0059] 2) 15 g of carotenoids and 4 g of antioxidant propyl gallic acid were mixed to obtain an oil phase b);
[0060] 3) adding the oil phase b) into the water phase a), mixing, stirring at a shearing speed of 6600prm, to obtain a mixed phase c);
[0061] 4) adding 6 g of crosslinking agent polymaleic acid (directly added) to the mixed phase c) in step 3), heating at 1400° C. for 18 h, and stirring to obtain emulsion d);
[0062] 5) spray drying the emulsion d) obtained in step 4) at a spray drying temperature of 84° C. and an atomizer speed of 32 Hz to obtain carotenoid microcapsules with a carotene particle size D50 of 280 μm and a carotene content of 4%.
[0063] Comparative Example 1
[0064] 1) Dissolve 40 g of sodium lignin sulfonate with a sulfonation degree of 30% in 60 g of water, heat to 60° C., stir at 2000 rpm until uniformly dispersed, and add 2 g of glucose as a filler to form an aqueous phase a);
[0065] 2) mixing 5 g of carotenoids with 2 g of antioxidant BHT to obtain an oil phase b);
[0066] 3) adding the oil phase b) into the water phase a), mixing, stirring at a shearing speed of 6000prm, to obtain a mixed phase c);
[0067] 4) adding 2 g of xanthan gum as a crosslinking agent (directly added) to the mixed phase c) in step 3), heating at 80° C. for 15 h, and stirring to obtain an emulsion d);
[0068] 5) spray drying the emulsion d) obtained in step 4) at a spray drying temperature of 80° C. and an atomizer speed of 30 Hz to obtain carotenoid microcapsules with a carotene particle size D50 of 214 μm and a carotene content of 8.36%.
[0069] Comparative Example 2
[0070] 1) Dissolve 25 g of sodium lignin sulfonate with a sulfonation degree of 40% in 60 g of water, heat to 60° C., stir at 2000 rpm until uniformly dispersed, and add 17 g of glucose as a filler to form an aqueous phase a);
[0071] 2) mixing 5 g of carotenoids with 2 g of antioxidant BHT to obtain an oil phase b);
[0072] 3) adding the oil phase b) into the water phase a), mixing, stirring at a shearing speed of 6000prm, to obtain a mixed phase c);
[0073] 4) adding 2 g of xanthan gum as a crosslinking agent (directly added) to the mixed phase c) in step 3), heating at 80° C. for 15 h, and stirring to obtain an emulsion d);
[0074] 5) spray drying the emulsion d) obtained in step 4) at a spray drying temperature of 80° C. and an atomizer speed of 30 Hz to obtain carotenoid microcapsules with a carotene particle size D50 of 248 μm and a carotene content of 8.5%.
[0075] Comparative Example 3
[0076] 1) Dissolve 40 g of sodium lignin sulfonate with a sulfonation degree of 40% in 60 g of water, heat to 60° C., stir at 2000 rpm until uniformly dispersed, and add 2 g of glucose as a filler to form an aqueous phase a);
[0077] 2) mixing 5 g of carotenoids with 2 g of antioxidant BHT to obtain an oil phase b);
[0078] 3) adding the oil phase b) into the water phase a), mixing, stirring at a shearing speed of 6000prm, to obtain a mixed phase c);
[0079] 4) adding 2 g of xanthan gum as a crosslinking agent (directly added) to the mixed phase c) in step 3), heating at 75° C. for 24 h, and stirring to obtain an emulsion d);
[0080] 5) spray drying the emulsion d) obtained in step 4) at a spray drying temperature of 80° C. and an atomizer speed of 30 Hz to obtain carotenoid microcapsules with a carotene particle size D50 of 318 μm and a carotene content of 9.4%.
[0081] Comparative Example 4
[0082] 1) Dissolve 40 g of sodium lignin sulfonate with a sulfonation degree of 40% in 60 g of water, heat to 60° C., stir at 2000 rpm until uniformly dispersed, and add 2 g of glucose as a filler to form an aqueous phase a);
[0083] 2) mixing 5 g of carotenoids with 2 g of antioxidant BHT to obtain an oil phase b);
[0084] 3) adding the oil phase b) into the water phase a), mixing, stirring at a shearing speed of 6000prm, to obtain a mixed phase c);
[0085] 4) heating the mixed phase c) in step 3) to 80° C. for a crosslinking time of 24 h and stirring to obtain an emulsion d);
[0086] 5) spray drying the emulsion d) obtained in step 4) at a spray drying temperature of 80° C. and an atomizer speed of 30 Hz to obtain carotenoid microcapsules with a carotene particle size D50 of 350 μm and a carotene content of 11.24%.
[0087] The hygroscopicity of the product was tested according to the "9103 Guidelines for Drug Hygroscopicity Test" of the "Chinese Pharmacopoeia" (2020 Edition). The results are shown in Table 1:
[0088] The product stability test was conducted in accordance with the Technical Guidelines for Stability Studies of Chemical Drugs (APIs and Preparations) (revised), and the results are shown in Table 1:
[0089]
[0090]
Claims
1. A carotenoid microcapsule preparation, which is prepared from the following raw materials in parts by weight: 5 to 20 parts of carotenoid, 40 to 80 parts of lignin sulfonate, 2 to 20 parts of filler, 2 to 10 parts of cross-linking agent, 2 to 5 parts of antioxidant, and 60 to 160 parts of water.
2. The carotenoid microcapsule preparation according to claim 1, characterized in that: The lignin sulfonate is a kind of sodium lignin sulfonate or calcium lignin sulfonate, with a molecular weight of 800-100000 and a sulfonation degree of 40-70%.
3. The carotenoid microcapsule preparation according to claim 1 or 2, characterized in that: The filler is selected from at least one of sucrose, maltose, glucose and syrup.
4. The carotenoid microcapsule preparation according to any one of claims 1 to 3, characterized in that: The cross-linking agent is selected from at least one of xanthan gum, carboxymethyl cellulose, methyl cellulose, polymaleic acid and succinic acid.
5. The carotenoid microcapsule preparation according to any one of claims 1 to 4, characterized in that: The antioxidant is selected from at least one of tocopherol, fatty acid ascorbic acid ester, butylated hydroxytoluene (BHT), butylated hydroxyanisole (BHA), propyl gallic acid, and tert-butylhydroxyquinoline.
6. The method for preparing the carotenoid microcapsule preparation according to any one of claims 1 to 5, characterized in that: The method comprises the following steps: 1) dissolving lignin sulfonate in water, heating, stirring until uniformly dispersed, and adding filler to form aqueous phase a); 2) mixing the carotenoids and the antioxidant to obtain an oil phase b); 3) adding the oil phase b) into the water phase a), mixing, shearing and stirring to obtain a mixed phase c); 4) adding a crosslinking agent to the mixed phase c) in step 3), heating and stirring to obtain an emulsion d); 5) spray drying the emulsion d) obtained in step 4) to obtain carotenoid microcapsules.
7. The preparation method according to claim 6, characterized in that: In step 1), the heating temperature is 60-65° C., the stirring speed is 2000-4000 rpm, and the stirring time is 10-120 min.
8. The preparation method according to claim 6 or 7, characterized in that: In step 3), the shearing speed is 6000-7000 rpm, and the shearing time is 10-90 min.
9. The preparation method according to any one of claims 6 to 8, characterized in that: The heating temperature in step 4) is 80° C. to 190° C.; the cross-linking time is 15 to 24 hours.
10. The preparation method according to any one of claims 6 to 9, characterized in that: In step 5), the spray drying temperature is 80-85° C. and the atomizer speed is 30-35 Hz.