High-stability lutein ester-vitamin C tabletted candy of blueberry leaf and preparation method thereof

Abstract

The present application relates to a kind of high stability blue leaf yellow ester vitamin C tablet candy and its preparation method, belong to functional food technical field.The tablet candy includes isomalt, blue powder, oligoisomaltose, xylitol, black currant powder, leaf yellow ester double-layer microcapsule powder, polydextrose, (3R, 3'S)-dihydroxy-β-carotene double-layer microcapsule powder, vitamin C, rosemary extract, citric acid, stevioside and magnesium stearate;The double-layer microcapsule powder includes active ingredient and ascorbic acid from inside to outside successively, the first wall material layer of sodium octenyl succinate starch and malt dextrin, and the second wall material layer of sodium alginate and chitosan;The tablet candy prepared by the present application has high stability, good bioavailability, and has good eye vision protection effect.

Description

Technical Field

[0001] This invention belongs to the field of functional food technology and relates to a highly stable blueberry lutein ester vitamin C compressed candy and its preparation method. Background Technology

[0002] With the widespread use of electronic products and changes in people's lifestyles, excessive eye strain has become a common phenomenon, and problems such as visual fatigue and vision decline are becoming increasingly prominent. Lutein esters, as an important carotenoid, are the main pigment components of the macular region of the retina and can effectively absorb blue light and protect the retina from oxidative damage. However, lutein esters are extremely sensitive to light, heat, and oxygen, and have poor stability. They are easily degraded and inactivated during processing and storage, which limits their application in food.

[0003] However, existing products still have the following shortcomings: First, the stability of lutein esters still needs to be further improved, and the active ingredients are lost significantly during long-term storage; second, the product formulas are relatively simple, and the synergistic effect between various active ingredients is not fully utilized; third, existing products mostly use sucrose, glucose, etc. as sweeteners, which have a high sugar content and are not suitable for diabetic patients and people who need to control their blood sugar.

[0004] Honeysuckle berries are a type of wild berry rich in anthocyanins. Honeysuckle berry anthocyanins have excellent antioxidant activity, with a scavenging rate of over 90% against DPPH free radicals. (3R,3'S)-dihydroxy-β-carotene is a new food ingredient that works synergistically with lutein esters to better protect the eyes. Vitamin C, as a powerful antioxidant, can effectively protect lutein esters from oxidative damage.

[0005] Therefore, there is an urgent need to develop a highly stable blueberry lutein ester vitamin C compressed candy and its preparation method. Summary of the Invention

[0006] To address the shortcomings of existing technologies, the present invention aims to provide a highly stable blueberry lutein ester vitamin C compressed candy and its preparation method.

[0007] The objective of this invention can be achieved through the following technical solutions: A highly stable blueberry lutein ester vitamin C compressed candy, the candy comprising the following ingredients in parts by weight: Isomalt 30-50 parts, honeysuckle berry powder 5-15 parts, isomaltose oligosaccharide 5-15 parts, xylitol 5-15 parts, blackcurrant powder 3-10 parts, lutein ester bilayer microcapsule powder 2-8 parts, polydextrose 3-10 parts, (3R,3'S)-dihydroxy-β-carotene bilayer microcapsule powder 0.5-3 parts, vitamin C 0.5-3 parts, rosemary extract 0.1-2 parts, citric acid 0.1-1 parts, steviol glycosides 0.05-0.5 parts, magnesium stearate 0.5-2 parts; The lutein ester bilayer microcapsule powder comprises, from the inside out, a core material, a first wall material layer, and a second wall material layer; the core material contains lutein ester and ascorbic acid; the first wall material layer contains sodium octenyl succinate starch and maltodextrin; and the second wall material layer contains sodium alginate and chitosan. The (3R,3'S)-dihydroxy-β-carotene bilayer microcapsule powder comprises, from the inside out, a core material, a first wall material layer, and a second wall material layer; the core material contains (3R,3'S)-dihydroxy-β-carotene and ascorbic acid; the first wall material layer contains sodium octenyl succinate starch and maltodextrin; and the second wall material layer contains sodium alginate and chitosan.

[0008] Furthermore, the rosemary extract contains 10% to 40% carrageenan by mass and 2% to 10% rosmarinic acid by mass.

[0009] Furthermore, in the lutein ester bilayer microcapsule powder, the mass ratio of the core material, the first wall material layer, and the second wall material layer is (10~20):(25~40):(10~20); the mass ratio of lutein ester to ascorbic acid in the core material is (5~15):(0.5~3).

[0010] Furthermore, in the (3R,3'S)-dihydroxy-β-carotene bilayer microcapsule powder, the mass ratio of the core material, the first wall material layer, and the second wall material layer is (5~15):(25~40):(10~20); and the mass ratio of (3R,3'S)-dihydroxy-β-carotene to ascorbic acid in the core material is (3~10):(0.5~3).

[0011] Furthermore, the mass ratio of sodium alginate to chitosan in the second wall material layer is (1~3):(1~2), the viscosity of sodium alginate is 200~500 mPa·s, and the degree of deacetylation of chitosan is 85%~95%.

[0012] Furthermore, the preparation method of the lutein ester bilayer microcapsule powder includes the following specific steps: S6-1: Mix lutein ester and ascorbic acid at a mass ratio of (5~15):(0.5~3), add sunflower seed oil at 0.5~2 times the mass of lutein ester as a solvent, stir at 60~80℃ for 10~30min; add purified water, and homogenize under high pressure at 50~70℃, with a homogenization pressure of 50~80MPa, homogenize 2~4 times to obtain the core material emulsion; S6-2: Dissolve sodium octenyl succinate starch and maltodextrin in purified water at a mass ratio of (1~3):(1~2), stir at 60~75℃ for 10~30 min, cool to 30~40℃, add core material emulsion, and emulsify by high-speed shearing for 15~30 min at a shear rate of 10000~18000 rpm to obtain the microcapsule emulsion embedded in the first wall material; S6-3: Dissolve sodium alginate in purified water to prepare a sodium alginate solution with a mass fraction of 0.5%~2%. Add the microcapsule emulsion embedded in the first wall material under stirring conditions, stir for 10~30 min, and add calcium chloride solution with a mass fraction of 1%~5% dropwise for cross-linking and solidification for 30~60 min. Then add chitosan solution and continue stirring for 20~40 min to obtain a double-layer embedded microcapsule emulsion. S6-4: The double-layer encapsulated microcapsule emulsion is spray-dried at an inlet air temperature of 150~180℃ and an outlet air temperature of 70~90℃ to obtain the lutein ester double-layer microcapsule powder.

[0013] Furthermore, the preparation method of the (3R,3'S)-dihydroxy-β-carotene bilayer microcapsule powder includes the following specific steps: S7-1: Mix (3R,3'S)-dihydroxy-β-carotene and ascorbic acid at a mass ratio of (3~10):(0.5~3), add purified water, stir at 40~55℃ for 10~30 min, adjust the pH to 6.5~7.5, and then grind and disperse to a particle size D. 90 ≤1μm; then high-pressure homogenization is performed at a pressure of 60~100MPa, and homogenization is performed 3~5 times to obtain the core material emulsion; S7-2: Dissolve sodium octenyl succinate starch and maltodextrin in purified water at a mass ratio of (1~3):(1~2), stir at 50~65℃ for 10~30 min, cool to 25~35℃, add the core material emulsion prepared in S7-1, and emulsify by high-speed shearing for 10~20 min at a shear rate of 8000~15000 rpm to obtain the microcapsule emulsion embedded in the first wall material; S7-3: Dissolve sodium alginate in purified water to prepare a sodium alginate solution with a mass fraction of 0.5%~2%. Add the microencapsulation emulsion prepared in S7-2 under stirring conditions, stir for 10~30 min, and add calcium chloride solution with a mass fraction of 1%~5% dropwise for cross-linking and solidification for 30~60 min. Then add chitosan solution and continue stirring for 20~40 min to obtain a double-layer embedded microencapsulation emulsion. S7-4: The double-layer encapsulated microcapsule emulsion obtained in S7-3 is spray-dried at an inlet air temperature of 140~170℃ and an outlet air temperature of 60~80℃ to obtain the (3R,3'S)-dihydroxy-β-carotene double-layer microcapsule powder.

[0014] A method for preparing highly stable honeysuckle lutein ester vitamin C compressed candy, the method comprising the following steps. S8-1: Weigh out the following ingredients according to the formula: isomalt, honeysuckle powder, isomaltose oligosaccharide, xylitol, blackcurrant powder, lutein ester bilayer microcapsule powder, polydextrose, (3R,3'S)-dihydroxy-β-carotene bilayer microcapsule powder, vitamin C, rosemary extract, citric acid, steviol glycosides, and magnesium stearate. Grind them separately and pass them through a 60-100 mesh sieve. S8-2: Add all raw materials except magnesium stearate into a mixer and mix for 10-30 minutes. Add a wetting agent to make a soft material. Granulate the material through a 16-20 mesh sieve and dry it at 40-55℃ until the moisture content of the particles is ≤5%. Then, granulate the material through a 14-20 mesh sieve. S8-3: Add the granulated granules and magnesium stearate into a mixer and mix for 5-15 minutes. Then, feed the mixed material into a tablet press and compress it into tablets to obtain the high-stability honeysuckle lutein ester vitamin C compressed candy.

[0015] Furthermore, the wetting agent in S8-2 is purified water or an ethanol solution with a volume fraction of 50% to 95%, and the amount of wetting agent added is 5% to 20% of the total mass of the raw materials.

[0016] Furthermore, in S8-3, the tableting environment temperature is 15~25℃, the tableting pressure is 10~30kN, and the tableting speed is 30~50rpm.

[0017] Lutein esters and (3R,3'S)-dihydroxy-β-carotene are both carotenoids, containing multiple conjugated double bonds in their molecular structures, making them susceptible to oxidative degradation under the influence of light, heat, and oxygen. This invention employs a double-layer microencapsulation structure to protect them.

[0018] Sodium octenyl succinate starch in the first wall material layer has good emulsifying and film-forming properties, and is a commonly used microencapsulation wall material in the food industry. Lutein microcapsules prepared with sodium octenyl succinate starch as the wall material have a high lutein content retention rate when placed at 25°C. Maltodextrin, as a filler and structural enhancer, further improves the integrity and density of the microcapsules.

[0019] The second wall layer utilizes a composite membrane formed by the polyelectrolyte complexation reaction of sodium alginate and chitosan. The chitosan-sodium alginate capsule, with its polyelectrolyte composite membrane, acts as a barrier between the active ingredient and the external environment, reducing the impact of adverse factors such as acids, alkalis, and enzymes on the active ingredient and effectively maintaining its stability. The polyelectrolyte reaction between sodium alginate and chitosan reduces the pore size of the sodium alginate network structure, thereby slowing the release rate of the active ingredient. Through the synergistic barrier effect of the double-layer wall material, the barrier performance against oxygen and water vapor is significantly improved compared to a single-layer wall material. Furthermore, the second wall layer exhibits excellent pH responsiveness, allowing the active ingredient to safely pass through the acidic environment of the stomach, avoiding destruction by gastric acid, and enabling efficient absorption after targeted release in the intestines, thus improving bioavailability.

[0020] This invention simultaneously encapsulates ascorbic acid within the core material of a double-layered microcapsule, achieving in-situ co-encapsulation of the antioxidant and the protected substance. As a potent antioxidant, ascorbic acid directly scavenges trace amounts of oxygen free radicals that infiltrate within the microcapsule, forming a close-fitting protection for lutein esters and (3R,3'S)-dihydroxy-β-carotene, further extending the shelf life of the active ingredients.

[0021] Sageric acid in rosemary extract possesses an ortho-dihydroxyl structure, enabling it to efficiently scavenge free radicals through a hydrogen atom transfer mechanism. Sageric acid exhibits outstanding thermal stability, overcoming the weakness of most natural antioxidants, such as vitamin C and tea polyphenols, which decompose at high temperatures. The antioxidant efficacy of rosemary extract surpasses that of existing natural antioxidants like vitamin C, vitamin E, and tea polyphenols. Sageric acid effectively scavenge free radicals and inhibit lipid peroxidation. This invention constructs a ternary synergistic antioxidant system of sageric acid, vitamin C, and honeysuckle anthocyanins. The phenolic acids in rosemary can synergistically work with vitamin-based antioxidants, thereby enhancing the overall antioxidant effect.

[0022] Blueberry anthocyanins possess multiple benefits, including protecting eyesight, scavenging free radicals, and chelating metal ions. Their eye-protecting mechanisms include activating retinal rhodopsin regeneration and inhibiting corneal epithelial cell apoptosis. Simultaneously, the potent antioxidant capacity of blueberry anthocyanins, combined with rosemary extract and vitamin C, forms a triple antioxidant defense. Anthocyanins chelate metal ions to inhibit free radical generation at its source, vitamin C scavenge free radicals already generated in the aqueous phase, and oxalic acid protects carotenoids in the oil phase from lipid peroxidation. These three components cover different mechanisms and phases of action, achieving comprehensive and multi-layered antioxidant effects.

[0023] The beneficial effects of this invention are: This invention utilizes a double-layer microencapsulation method to encapsulate lutein esters and (3R,3'S)-dihydroxy-β-carotene within double-layer microcapsules made of sodium octenyl succinate starch / maltodextrin as the first wall material and sodium alginate / chitosan as the second wall material, respectively, using targeted and optimized process parameters. The outer sodium alginate-chitosan polyelectrolyte composite membrane forms a dense physical barrier, significantly improving the storage stability of the active ingredients, and also imparts pH-responsive intestinal-targeted release properties, effectively enhancing bioavailability. Simultaneously, the core material... The encapsulated ascorbic acid provides in-situ antioxidant protection. The rosemary extract added to the formula, together with vitamin C and honeysuckle anthocyanins, forms a fat-soluble and water-soluble synergistic antioxidant network, achieving comprehensive free radical scavenging and metal ion chelation. In addition, the product uses sugar substitutes such as isomaltitol, isomaltooligosaccharide, and xylitol as sweeteners, without adding sucrose. The content of each active ingredient complies with national food safety limits, making it suitable for a wide range of people. Moreover, the preparation process parameters are clear and controllable, and industrial production can be achieved using conventional equipment. Attached Figure Description

[0024] To facilitate understanding by those skilled in the art, the present invention will be further described below with reference to the accompanying drawings.

[0025] Figure 1 The diagram shows the apoptotic phenotypes of zebrafish eye cells in Example 1, the model group, and the control group of this invention. The yellow dashed area represents the eye, and the green dots represent apoptotic cells. Figure 2 These are pathological sections of apoptotic cells in the eyes of the model group and control group in Example 1 of this invention, with red arrows pointing to apoptotic cells. Detailed Implementation

[0026] To further illustrate the technical means and effects of the present invention in achieving the intended purpose, the following detailed description of the specific implementation methods, structures, features and effects of the present invention, in conjunction with the accompanying drawings and preferred embodiments, is provided.

[0027] It should be noted that, unless otherwise specified, the present invention does not specifically limit the source of the raw materials used in the following embodiments. Commercially available products or products prepared by conventional preparation methods that are well known to those skilled in the art can be used. Experimental methods that do not specify specific conditions are all conventional methods and conventional conditions well known in the art.

[0028] Example 1

[0029] This embodiment provides a highly stable blueberry lutein ester vitamin C compressed candy, comprising the following raw materials in parts by weight: 40 parts isomaltitol, 10 parts honeysuckle berry powder, 10 parts isomaltose oligosaccharide, 10 parts xylitol, 6 parts blackcurrant powder, 5 parts lutein ester bilayer microcapsule powder, 6 parts polydextrose, 1.5 parts (3R,3'S)-dihydroxy-β-carotene bilayer microcapsule powder, 1.5 parts vitamin C, 0.6 parts rosemary extract, 0.5 parts citric acid, 0.2 parts steviol glycosides, and 1 part magnesium stearate.

[0030] The rosemary extract contains 25% caryopsisic acid and 5% rosmarinic acid. The honeysuckle berry powder contains 28% anthocyanins. Each compressed candy weighs 0.7g, and the daily intake should not exceed 4 tablets.

[0031] Preparation of lutein ester bilayer microcapsule powder: The mass ratio of the core material, the first wall material layer, and the second wall material layer is 15:35:15; the mass ratio of lutein ester to ascorbic acid in the core material is 10:2; the mass ratio of sodium alginate to chitosan in the second wall material layer is 2:1; the viscosity of sodium alginate is 350 mPa·s; and the degree of deacetylation of chitosan is 90%.

[0032] S6-1: Lutein ester and ascorbic acid are mixed at a mass ratio of 10:2. Sunflower seed oil with a mass of 1 times that of lutein ester is added as a solvent. The mixture is stirred at 70°C for 20 min. Purified water is added. The mixture is homogenized under high pressure at 60°C with a homogenization pressure of 65 MPa for 3 times to obtain the core material emulsion. S6-2: Dissolve sodium octenyl succinate starch and maltodextrin in purified water at a mass ratio of 2:1, stir at 68℃ for 20 min, cool to 35℃, add core material emulsion, and emulsify by high-speed shearing for 20 min at a shear rate of 14000 rpm to obtain the microcapsule emulsion embedded in the first wall material. S6-3: Dissolve sodium alginate in purified water to prepare a 1% sodium alginate solution. Add the microcapsule emulsion embedded in the first wall material under stirring conditions, stir for 20 min, and then add a 3% calcium chloride solution for cross-linking and curing for 45 min. Then add chitosan solution (chitosan dissolved in a 2% acetic acid solution to prepare a 1% chitosan solution), and continue stirring for 30 min to obtain a double-layer embedded microcapsule emulsion. S6-4: The double-layer encapsulated microcapsule emulsion is spray-dried at an inlet air temperature of 165°C and an outlet air temperature of 80°C to obtain the lutein ester double-layer microcapsule powder.

[0033] Preparation of (3R,3'S)-dihydroxy-β-carotene bilayer microcapsule powder: The mass ratio of the core material, the first wall material layer, and the second wall material layer is 10:35:15; the mass ratio of (3R,3'S)-dihydroxy-β-carotene to ascorbic acid in the core material is 8:2; the mass ratio of sodium alginate to chitosan in the second wall material layer is 2:1, the viscosity of sodium alginate is 350 mPa·s, and the degree of deacetylation of chitosan is 90%.

[0034] S7-1: (3R,3'S)-dihydroxy-β-carotene and ascorbic acid were mixed at a mass ratio of 8:2, purified water was added, and the mixture was stirred at 48℃ for 20 min. The pH was adjusted to 7.0, and the mixture was then ground and dispersed until the particle size D90 ≤ 1 μm. Subsequently, high-pressure homogenization was performed at a pressure of 80 MPa for 4 times to obtain the core material emulsion. S7-2: Dissolve sodium octenyl succinate starch and maltodextrin in purified water at a mass ratio of 2:1, stir at 58℃ for 20 min, cool to 30℃, add the core material emulsion prepared in S7-1, and emulsify by high-speed shearing for 15 min at a shear rate of 12000 rpm to obtain the microcapsule emulsion embedded in the first wall material. S7-3: Dissolve sodium alginate in purified water to prepare a 1% sodium alginate solution. Add the microcapsule emulsion prepared in S7-2 under stirring conditions and stir for 20 min. Add a 3% calcium chloride solution for cross-linking and solidification for 45 min. Then add chitosan solution (chitosan dissolved in a 2% acetic acid solution to prepare a 1% chitosan solution) and continue stirring for 30 min to obtain a double-layer embedded microcapsule emulsion. S7-4: The double-layer encapsulated microcapsule emulsion prepared in S7-3 is spray-dried at an inlet air temperature of 155°C and an outlet air temperature of 70°C to obtain the (3R,3'S)-dihydroxy-β-carotene double-layer microcapsule powder.

[0035] Preparation of compressed candy: S8-1: Weigh out the following ingredients according to the formula: isomalt, honeysuckle powder, isomaltose oligosaccharide, xylitol, blackcurrant powder, lutein ester bilayer microcapsule powder, polydextrose, (3R,3'S)-dihydroxy-β-carotene bilayer microcapsule powder, vitamin C, rosemary extract, citric acid, steviol glycosides, and magnesium stearate. Grind them separately and pass them through an 80-mesh sieve. S8-2: Add all raw materials except magnesium stearate into a mixer and mix for 20 minutes. Add 10% of the total mass of the raw materials of purified water as a wetting agent to make a soft material. Granulate it through an 18-mesh sieve and dry it at 50℃ until the moisture content of the particles is ≤5%. Then, granulate it through a 16-mesh sieve. S8-3: The granulated particles and magnesium stearate are put into a mixer and mixed for 10 minutes. The mixed material is then fed into a tableting machine. The tableting environment temperature is 20℃, the tableting pressure is 20kN, and the tableting speed is 40rpm. The tablets are compressed into tablets with a weight of 0.7g each, thus obtaining the high-stability honeysuckle lutein ester vitamin C compressed candy.

[0036] Example 2

[0037] This embodiment provides a highly stable blueberry lutein ester vitamin C compressed candy, comprising the following raw materials in parts by weight: 30 parts isomaltitol, 5 parts honeysuckle berry powder, 5 parts isomaltose oligosaccharide, 5 parts xylitol, 3 parts blackcurrant powder, 2 parts lutein ester bilayer microcapsule powder, 30 parts polydextrose, 0.5 parts (3R,3'S)-dihydroxy-β-carotene bilayer microcapsule powder, 0.5 parts vitamin C, 0.1 parts rosemary extract, 0.1 parts citric acid, 0.05 parts steviol glycosides, and 0.5 parts magnesium stearate; The remaining raw materials and preparation methods are the same as in Example 1.

[0038] Example 3

[0039] This embodiment provides a highly stable blueberry lutein ester vitamin C compressed candy, comprising the following raw materials in parts by weight: 35 parts isomaltitol, 7 parts honeysuckle fruit powder, 7 parts isomaltose oligosaccharide, 7 parts xylitol, 5 parts blackcurrant powder, 4 parts lutein ester bilayer microcapsule powder, 5 parts polydextrose, 1 part (3R,3'S)-dihydroxy-β-carotene bilayer microcapsule powder, 1 part vitamin C, 0.3 parts rosemary extract, 0.3 parts citric acid, 0.1 parts steviol glycoside, 0.8 parts magnesium stearate; The remaining raw materials and preparation methods are the same as in Example 1.

[0040] Example 4

[0041] This embodiment provides a highly stable blueberry lutein ester vitamin C compressed candy, comprising the following raw materials in parts by weight: 45 parts isomaltitol, 12 parts honeysuckle berry powder, 12 parts isomaltose oligosaccharide, 12 parts xylitol, 8 parts blackcurrant powder, 6 parts lutein ester bilayer microcapsule powder, 8 parts polydextrose, 2 parts (3R,3'S)-dihydroxy-β-carotene bilayer microcapsule powder, 2 parts vitamin C, 1 part rosemary extract, 0.7 parts citric acid, 0.3 parts steviol glycosides, and 1.5 parts magnesium stearate; The remaining raw materials and preparation methods are the same as in Example 1.

[0042] Example 5

[0043] This embodiment provides a highly stable blueberry lutein ester vitamin C compressed candy, comprising the following raw materials in parts by weight: 50 parts isomaltitol, 15 parts honeysuckle berry powder, 15 parts isomaltose oligosaccharide, 15 parts xylitol, 10 parts blackcurrant powder, 8 parts lutein ester bilayer microcapsule powder, 10 parts polydextrose, 3 parts (3R,3'S)-dihydroxy-β-carotene bilayer microcapsule powder, 3 parts vitamin C, 2 parts rosemary extract, 1 part citric acid, 0.5 parts steviol glycoside, 2 parts magnesium stearate; The remaining raw materials and preparation methods are the same as in Example 1.

[0044] Example 6

[0045] The difference between this embodiment and Embodiment 1 is that: in the preparation of the lutein ester bilayer microcapsule powder, the mass ratio of the core material, the first wall material layer, and the second wall material layer is 18:32:18; the mass ratio of lutein ester to ascorbic acid in the core material is 8:1; and the mass ratio of sodium alginate to chitosan in the second wall material layer is 2.5:1. In the preparation of (3R,3'S)-dihydroxy-β-carotene bilayer microcapsule powder, the mass ratio of the core material, the first wall material layer, and the second wall material layer is 12:32:18; the mass ratio of (3R,3'S)-dihydroxy-β-carotene to ascorbic acid in the core material is 6:1.5. The remaining raw materials and preparation methods are the same as in Example 1.

[0046] Example 7

[0047] The difference between this embodiment and Embodiment 1 is that: in the preparation of the lutein ester bilayer microcapsule powder, the mass ratio of the core material, the first wall material layer and the second wall material layer is 12:38:12; the mass ratio of lutein ester to ascorbic acid in the core material is 12:3; and the mass ratio of sodium alginate to chitosan in the second wall material layer is 1.5:1. In the preparation of (3R,3'S)-dihydroxy-β-carotene bilayer microcapsule powder, the mass ratio of the core material, the first wall material layer, and the second wall material layer is 8:38:12; the mass ratio of (3R,3'S)-dihydroxy-β-carotene to ascorbic acid in the core material is 10:3; and the mass ratio of sodium alginate to chitosan in the second wall material layer is 1.5:1. The remaining raw materials and preparation methods are the same as in Example 1.

[0048] Comparative Example 1 The difference between this comparative example and Example 1 is that rosemary extract is not added, the amount of vitamin C is adjusted to 1.5 parts, and the other raw materials and preparation methods are the same as in Example 1.

[0049] Comparative Example 2 The difference between this comparative example and Example 1 is that the lutein ester microcapsule powder and (3R,3'S)-dihydroxy-β-carotene microcapsule powder are only encapsulated in the first wall material layer (sodium octenyl succinate starch + maltodextrin), without encapsulation in the second wall material layer of sodium alginate-chitosan. The other raw materials and preparation methods are the same as in Example 1.

[0050] Comparative Example 3 The difference between this comparative example and Example 1 is that the lutein ester microcapsule powder and (3R,3'S)-dihydroxy-β-carotene microcapsule powder are only encapsulated in the second wall material layer (sodium alginate-chitosan), without encapsulation in the first wall material layer (sodium octenyl succinate starch + maltodextrin). The other raw materials and preparation methods are the same as in Example 1.

[0051] Comparative Example 4 The difference between this comparative example and Example 1 is that lutein ester and (3R,3'S)-dihydroxy-β-carotene were prepared using the exact same microencapsulation process parameters, both following the process parameters for lutein ester in Example 1. The remaining raw materials and preparation methods were the same as in Example 1.

[0052] Comparative Example 5 The difference between this comparative example and Example 1 is that lutein ester and (3R,3'S)-dihydroxy-β-carotene were prepared using the exact same microencapsulation process parameters, both following the process parameters for (3R,3'S)-dihydroxy-β-carotene in Example 1. The remaining raw materials and preparation methods were the same as in Example 1.

[0053] Comparative Example 6 The difference between this comparative example and Example 1 is that lutein ester and (3R,3'S)-dihydroxy-β-carotene are not microencapsulated, while the other raw materials and preparation methods are the same as in Example 1.

[0054] Eye vision protection test Test principle: The blood vessel structure in the zebrafish eye is very similar to that in humans, and the retinal structure of zebrafish is also highly similar to that of humans. Mycophenolate mofetil can induce apoptosis in zebrafish eye cells, mimicking human eye diseases. Using specific fluorescent staining (which appears green), apoptosis of eye cells in zebrafish with eye diseases is significantly increased compared to normal zebrafish, which can be observed under a fluorescence microscope.

[0055] Experimental Procedure: The zebrafish were divided into three groups: a normal control group, a model control group, and an eye protectant group. The normal control group did not ingest mycophenolate mofetil, while the model control group and the eye protectant group both ingested an equal amount of mycophenolate mofetil (which was dissolved in the aquaculture water). The eye protectant group ingested an eye protectant (specifically, the honeysuckle lutein ester vitamin C tablets prepared in Example 1) concurrently with mycophenolate mofetil. The honeysuckle lutein ester vitamin C tablets were dissolved in the aquaculture water. After a period of time, apoptosis-specific staining was performed on the zebrafish to observe apoptosis, and pathological sections were prepared to observe changes in the eye's pathological structure.

[0056] Depend on Figure 1 It can be seen that the number of apoptotic cells in the model control group was significantly higher than that in the normal control group, while the number of apoptotic cells in the eye protectant group (the blue honeysuckle lutein ester vitamin C compressed candy prepared in Example 1) was similar to that in the normal cells.

[0057] from Figure 2 Pathological sections also show that the model control group has more apoptotic cells, which are characterized by cell shrinkage and chromatin marginalization, while the cells in the eye protectant group (blue honeysuckle lutein ester vitamin C compressed candy prepared in Example 1) are morphologically similar to those in normal zebrafish.

[0058] Accelerated stability test Each sample was placed in a constant temperature and humidity chamber at 40℃±2℃ and 75%±5% relative humidity. Samples were taken and tested in 0 months, 3 months and 6 months respectively. Three samples were taken from each group at each time point, and the average value of the test results was taken.

[0059] Lutein ester content determination: Refer to GB 5009.248-2016 standard. Chromatographic conditions: Column: C30 column (4.6mm×250mm, 5μm), mobile phase: methanol-water (gradient elution), detection wavelength: 445nm, flow rate: 1.0mL / min, column temperature: 30℃, injection volume: 20μL.

[0060] Sample preparation: Take 20 compressed candies, grind them into fine powder, accurately weigh the powder equivalent to about 5 mg of lutein ester, place it in a stoppered conical flask, add 50 mL of n-hexane-anhydrous ethanol-acetone (2:1:1) mixed solvent, extract by ultrasonication for 15 min, filter, take the filtrate and filter it through a 0.45 μm microporous membrane before injection for analysis.

[0061] (3R, 3'S)-Dihydroxy-β-carotene content determination: Refer to GB / T 5009.83-2003 standard. Chromatographic conditions: Column: C30 column (4.6 mm × 250 mm, 5 μm), mobile phase: methanol-acetonitrile-water (gradient elution), detection wavelength: 450 nm, flow rate: 1.0 mL / min, column temperature: 30 ℃, injection volume: 20 μL.

[0062] Sample preparation: Same as lutein ester sample preparation method.

[0063] Retention rate calculation: Retention rate (%) = (C n / C0) × 100%, where C0 is the content of active ingredients at month 0, C n This represents the content of the active ingredient in month n.

[0064]

[0065] Based on the test data above, we can draw the following conclusions: After 6 months of storage, Examples 1-7 showed that the lutein ester retention rate was over 93.8%, and the (3R,3'S)-dihydroxy-β-carotene retention rate was over 92.8%, significantly better than the comparative examples. This result is attributed to the dual-protection system of physical barrier and chemical antioxidant system of rosemary extract constructed in this invention: the first wall layer forms a dense initial protective layer through emulsification and embedding, effectively isolating oxygen and water vapor from direct contact with the core material; the second wall layer forms a highly dense cross-linked network structure through the electrostatic interaction between sodium alginate and chitosan, further reducing the permeation rate of oxygen and water vapor, thus improving the barrier performance of the wall material compared to a single-layer wall material. Simultaneously, oxalic acid in the rosemary extract, as a highly efficient fat-soluble antioxidant, directly scavenges trace amounts of oxygen free radicals infiltrated in the oil phase, constructing a fat-soluble-water-soluble synergistic antioxidant network with ascorbic acid and honeysuckle anthocyanins embedded in the core material, achieving a synergistic effect of physical barrier and chemical antioxidant.

[0066] After 6 months of storage, the retention rate of lutein esters in Comparative Example 1 was 76.3%, which was 18.5 percentage points lower than that in Example 1; the retention rate of (3R,3'S)-dihydroxy-β-carotene was 19.9 percentage points lower than that in Example 1. This indicates that oxalic acid in rosemary extract plays an irreplaceable role in the synergistic antioxidant network. Oxalic acid has an ortho-dihydroxy structure, which can efficiently scavenge free radicals through a hydrogen atom transfer mechanism. At the same time, oxalic acid is an excellent fat-soluble antioxidant, forming a fully oil-water phase-covering antioxidant network with vitamin C: oxalic acid directly protects lutein esters and (3R,3'S)-dihydroxy-β-carotene in the oil phase, while vitamin C scavenge free radicals in the aqueous phase. The two regenerate each other through redox cycles, resulting in a significant improvement in overall antioxidant efficiency. Comparative Example 1, lacking rosemary extract, relies solely on vitamin C and honeysuckle anthocyanins to function in the aqueous phase, which cannot provide sufficient antioxidant protection for carotenoids in the oil phase, thus resulting in a decreased retention rate.

[0067] After 6 months of storage, the lutein ester retention rate of Comparative Example 2 was 60.5%, which was 34.3 percentage points lower than that of Example 1; the retention rate of (3R,3'S)-dihydroxy-β-carotene was 36.1 percentage points lower than that of Example 1. Although the single-layer wall material can form a preliminary emulsion embedding, the wall material has limited thickness and insufficient density. During long-term storage, oxygen and water vapor can still slowly penetrate through the wall material and reach the surface of the core material, causing oxidative degradation.

[0068] After 6 months of storage, Comparative Example 3 showed a lutein ester retention rate of 54.0% and a (3R,3'S)-dihydroxy-β-carotene retention rate of 51.2%, even lower than Comparative Example 2. Since both lutein ester and (3R,3'S)-dihydroxy-β-carotene are fat-soluble / weakly polar compounds, they are difficult to form a stable dispersion system in sodium alginate aqueous solution. The core material, without sodium octenyl succinate starch emulsification, could not be effectively encapsulated by sodium alginate-chitosan. During spray drying, a large amount of active ingredients were exposed to hot air and degraded, resulting in an initial encapsulation rate far lower than that of Example 1. Therefore, although the retention rate of Comparative Example 3 was calculated based on the measured content at month 0, the measured content at month 0 itself was already far lower than the theoretical value due to losses during the encapsulation process. This proves that the emulsification and embedding of the first wall material layer is a prerequisite for achieving efficient encapsulation. The second wall material layer is a functional enhancement layer based on the first wall material layer. The first wall material layer ensures that the core material is effectively encapsulated to form a stable microcapsule core. The second wall material layer provides additional dense barrier and pH-responsive release functions on this basis. The two work together and neither can be dispensed with.

[0069] After 6 months of storage, Comparative Example 4 showed a lutein ester retention rate of 83.6% and a (3R,3'S)-dihydroxy-β-carotene retention rate of 81.9%. In Comparative Example 5, after 6 months of storage, the retention rates for both were 86.2% and 84.3%, respectively, both lower than in Example 1. This indicates that lutein ester and (3R,3'S)-dihydroxy-β-carotene have significantly different physicochemical properties. Microencapsulation process parameters must be optimized separately for each of their characteristics. A uniform process cannot simultaneously meet the protection requirements of both active ingredients. Differentiated preparation is a necessary technical means to ensure optimal protection for both.

[0070] After 6 months of storage, Comparative Example 6 showed a lutein ester retention rate of only 35.2% and a (3R,3'S)-dihydroxy-β-carotene retention rate of only 30.4%, significantly lower than that of Example 1. This is because the unencapsulated active ingredients exist in free form within the compressed candy matrix, directly exposed to environmental factors such as oxygen, light, and moisture, resulting in rapid oxidative degradation. This further demonstrates the core role of microencapsulation in protecting active ingredients, as the wall material physically isolates the active ingredients from the external environment, significantly slowing down the rate of oxidative degradation.

[0071] The above description is merely a preferred embodiment of the present invention and is not intended to limit the present invention in any way. Although the present invention has been disclosed above with reference to preferred embodiments, it is not intended to limit the present invention. Any person skilled in the art can make some modifications or alterations to the above-disclosed technical content to create equivalent embodiments without departing from the scope of the present invention. Any brief modifications, equivalent changes and alterations made to the above embodiments based on the technical essence of the present invention without departing from the scope of the present invention shall still fall within the scope of the present invention.

Claims

1. A highly stable blueberry lutein ester vitamin C compressed candy, characterized in that, The candy comprises the following ingredients in parts by weight: Isomalt 30-50 parts, honeysuckle berry powder 5-15 parts, isomaltose oligosaccharide 5-15 parts, xylitol 5-15 parts, blackcurrant powder 3-10 parts, lutein ester bilayer microcapsule powder 2-8 parts, polydextrose 3-10 parts, (3R,3'S)-dihydroxy-β-carotene bilayer microcapsule powder 0.5-3 parts, vitamin C 0.5-3 parts, rosemary extract 0.1-2 parts, citric acid 0.1-1 parts, steviol glycosides 0.05-0.5 parts, magnesium stearate 0.5-2 parts; The lutein ester bilayer microcapsule powder comprises, from the inside out, a core material, a first wall material layer, and a second wall material layer; the core material contains lutein ester and ascorbic acid; the first wall material layer contains sodium octenyl succinate starch and maltodextrin; and the second wall material layer contains sodium alginate and chitosan. The (3R,3'S)-dihydroxy-β-carotene bilayer microcapsule powder comprises, from the inside out, a core material, a first wall material layer, and a second wall material layer; the core material contains (3R,3'S)-dihydroxy-β-carotene and ascorbic acid; the first wall material layer contains sodium octenyl succinate starch and maltodextrin; and the second wall material layer contains sodium alginate and chitosan.

2. The highly stable honeysuckle lutein ester vitamin C compressed candy according to claim 1, characterized in that, The rosemary extract contains 10% to 40% carrageenan by mass and 2% to 10% rosmarinic acid by mass.

3. The highly stable honeysuckle lutein ester vitamin C compressed candy according to claim 1, characterized in that, In the lutein ester bilayer microcapsule powder, the mass ratio of the core material, the first wall material layer and the second wall material layer is (10~20):(25~40):(10~20); the mass ratio of lutein ester to ascorbic acid in the core material is (5~15):(0.5~3).

4. The highly stable honeysuckle lutein ester vitamin C compressed candy according to claim 1, characterized in that, In the (3R,3'S)-dihydroxy-β-carotene bilayer microcapsule powder, the mass ratio of the core material, the first wall material layer, and the second wall material layer is (5~15):(25~40):(10~20); the mass ratio of (3R,3'S)-dihydroxy-β-carotene to ascorbic acid in the core material is (3~10):(0.5~3).

5. The highly stable blueberry lutein ester vitamin C compressed candy according to claim 1, characterized in that, The mass ratio of sodium alginate to chitosan in the second wall material layer is (1~3):(1~2), the viscosity of sodium alginate is 200~500 mPa·s, and the degree of deacetylation of chitosan is 85%~95%.

6. The highly stable honeysuckle lutein ester vitamin C compressed candy according to claim 1, characterized in that, The preparation method of the lutein ester bilayer microcapsule powder includes the following specific steps: S6-1: Mix lutein ester and ascorbic acid at a mass ratio of (5~15):(0.5~3), add sunflower seed oil at 0.5~2 times the mass of lutein ester as a solvent, stir at 60~80℃ for 10~30min; add purified water, and homogenize under high pressure at 50~70℃, with a homogenization pressure of 50~80MPa, homogenize 2~4 times to obtain the core material emulsion; S6-2: Dissolve sodium octenyl succinate starch and maltodextrin in purified water at a mass ratio of (1~3):(1~2), stir at 60~75℃ for 10~30 min, cool to 30~40℃, add core material emulsion, and emulsify by high-speed shearing for 15~30 min at a shear rate of 10000~18000 rpm to obtain the microcapsule emulsion embedded in the first wall material; S6-3: Dissolve sodium alginate in purified water to prepare a sodium alginate solution with a mass fraction of 0.5%~2%. Add the microcapsule emulsion embedded in the first wall material under stirring conditions, stir for 10~30 min, and add calcium chloride solution with a mass fraction of 1%~5% dropwise for cross-linking and solidification for 30~60 min. Then add chitosan solution and continue stirring for 20~40 min to obtain a double-layer embedded microcapsule emulsion. S6-4: The double-layer encapsulated microcapsule emulsion is spray-dried at an inlet air temperature of 150~180℃ and an outlet air temperature of 70~90℃ to obtain the lutein ester double-layer microcapsule powder.

7. The highly stable honeysuckle lutein ester vitamin C compressed candy according to claim 1, characterized in that, The preparation method of the (3R,3'S)-dihydroxy-β-carotene bilayer microcapsule powder includes the following specific steps: S7-1: Mix (3R,3'S)-dihydroxy-β-carotene and ascorbic acid at a mass ratio of (3~10):(0.5~3), add purified water, stir at 40~55℃ for 10~30 min, adjust the pH to 6.5~7.5, and then grind and disperse to a particle size D. 90 ≤1μm; then high-pressure homogenization is performed at a pressure of 60~100MPa, and homogenization is performed 3~5 times to obtain the core material emulsion; S7-2: Dissolve sodium octenyl succinate starch and maltodextrin in purified water at a mass ratio of (1~3):(1~2), stir at 50~65℃ for 10~30 min, cool to 25~35℃, add the core material emulsion prepared in S7-1, and emulsify by high-speed shearing for 10~20 min at a shear rate of 8000~15000 rpm to obtain the microcapsule emulsion embedded in the first wall material; S7-3: Dissolve sodium alginate in purified water to prepare a sodium alginate solution with a mass fraction of 0.5%~2%. Add the microencapsulation emulsion prepared in S7-2 under stirring conditions, stir for 10~30 min, and add calcium chloride solution with a mass fraction of 1%~5% dropwise for cross-linking and solidification for 30~60 min. Then add chitosan solution and continue stirring for 20~40 min to obtain a double-layer embedded microencapsulation emulsion. S7-4: The double-layer encapsulated microcapsule emulsion obtained in S7-3 is spray-dried at an inlet air temperature of 140~170℃ and an outlet air temperature of 60~80℃ to obtain the (3R,3'S)-dihydroxy-β-carotene double-layer microcapsule powder.

8. A method for preparing a highly stable blueberry lutein ester vitamin C compressed candy as described in any one of claims 1 to 7, characterized in that, The preparation method includes the following steps. S8-1: Weigh out the following ingredients according to the formula: isomalt, honeysuckle powder, isomaltose oligosaccharide, xylitol, blackcurrant powder, lutein ester bilayer microcapsule powder, polydextrose, (3R,3'S)-dihydroxy-β-carotene bilayer microcapsule powder, vitamin C, rosemary extract, citric acid, steviol glycosides, and magnesium stearate. Grind them separately and pass them through a 60-100 mesh sieve. S8-2: Add all raw materials except magnesium stearate into a mixer and mix for 10-30 minutes. Add a wetting agent to make a soft material. Granulate the material through a 16-20 mesh sieve and dry it at 40-55℃ until the moisture content of the particles is ≤5%. Then, granulate the material through a 14-20 mesh sieve. S8-3: Add the granulated granules and magnesium stearate into a mixer and mix for 5-15 minutes. Then, feed the mixed material into a tablet press and compress it into tablets to obtain the high-stability honeysuckle lutein ester vitamin C compressed candy.

9. The preparation method of a highly stable honeysuckle lutein ester vitamin C compressed candy according to claim 8, characterized in that, The wetting agent in S8-2 is purified water or an ethanol solution with a volume fraction of 50% to 95%, and the amount of wetting agent added is 5% to 20% of the total mass of the raw materials.

10. The preparation method of a highly stable honeysuckle lutein ester vitamin C compressed candy according to claim 8, characterized in that, The tableting environment temperature in S8-3 is 15~25℃, the tableting pressure is 10~30kN, and the tableting speed is 30~50rpm.

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