A highly active composition for resisting blue light damage and its preparation method

Abstract

The present invention provides a highly active composition for resisting blue light damage and a preparation method thereof. The composition includes lutein ester and zeaxanthin; the mass ratio of the lutein ester to zeaxanthin is 1:(0.8-1.5); the lutein ester is added in the form of lutein ester microcapsule powder; and the raw materials of the lutein ester microcapsule powder do not contain other oil components except lutein ester crystals. The present invention combines lutein ester and zeaxanthin to have good antioxidant and blue light damage resistance effects; the raw material lutein ester microcapsule powder used in the present invention solves the instability problem caused by high-temperature melting of lutein ester during the preparation process, effectively avoiding the problem of high-temperature sterilization instability or floating precipitation of the lutein ester microcapsule powder during application.

Description

Technical Field

[0001] The present invention belongs to the technical field of carotenoid preparation, and particularly relates to a composition with high activity for resisting blue light damage and a preparation method thereof. Background Art

[0002] Lutein esters are high-content lutein ester crystals derived from marigold flowers through a process of dehydration, crushing, and solvent extraction. They offer unique eye-protecting properties, preventing UV damage and acting as a strong oxidant to inhibit reactive oxygen free radicals, contributing to skincare, heart health, and immune enhancement. my country's Ministry of Health Announcement No. 12 of 2008 officially approved lutein esters as a new functional food resource.

[0003] Currently, lutein esters are primarily used in functional foods and dietary supplements for eye protection, primarily in the form of tablets and solid beverages. However, due to the inherent instability of lutein esters, a growing focus has emerged on their encapsulation. Lutein esters, whose main component is lutein dipalmitate, are solid at room temperature but have a relatively low melting point, softening above 50°C and melting at 60°C. Consequently, traditional encapsulation processes typically involve melting vegetable oil and lutein ester crystals, emulsifying the lutein esters and then encapsulating them with a wall material to produce microencapsulated lutein ester products. However, this process not only requires a carrier vegetable oil, reducing the loading capacity of the original lutein ester crystals, but also requires a high-temperature melting step, which can lead to degradation of the lutein esters and hinder the development of high-content products. Alternatively, solvents can be used to dissolve the lutein esters in place of vegetable oils, followed by solvent removal, addressing both of these issues. However, the introduction of solvents undoubtedly places pressure on the environment, and residual solvents pose safety concerns during administration.

[0004] Due to the unique properties of lutein ester crystal raw materials, the high-temperature melting or solvent method used in the existing technology when preparing lutein ester powder and microparticles by microencapsulation technology cannot produce high-content lutein ester microencapsulated products. At the same time, due to the high temperature process, not only does the lutein ester degrade during processing, but the stability of the microencapsulated product is also poor during subsequent storage.

[0005] CN113842434A discloses a lutein microcapsule powder composition and its application. The composition comprises the following components, by weight: 0.5-4 parts lutein, 10-40 parts seabuckthorn, 25-100 parts astragalus, 15-60 parts dendrobium, and 12-60 parts wolfberry. The synergistic effects of lutein, seabuckthorn, astragalus, dendrobium, and wolfberry significantly alleviate visual fatigue. The lutein microcapsule powder exhibits excellent thermal stability and can be used in a variety of dosage forms, including soft candies, beverages, compressed candies, and effervescent tablets. It is convenient to consume and carry, expanding the application of lutein in health foods.

[0006] CN109645201A discloses a composition containing lutein and lutein esters, a lutein tablet candy, and a preparation method and application thereof. The composition comprises lutein, lutein esters, zeaxanthin, blueberry powder, natural carotene, trehalose, and D-mannitol. The composition is used to prepare lutein tablet candy. The preparation method comprises: embedding natural carotene and the like, then mixing with the remaining materials except trehalose and D-mannitol, crushing, and sieving to obtain a powder; using the powder as the core material, coating and granulating with a wall material solution, drying, tableting, and coating to obtain the product. By combining specific components and contents, the amount absorbed by the human body can be met, and the components play a good synergistic role in eye protection. Through a specific process, the product is stable and has a sustained-release function, allowing people to effectively and continuously absorb the active ingredients, solving the problem of localized absorption.

[0007] CN116392461A A lutein composition comprising selective isomers of trans-R,R lutein and trans-R,R zeaxanthin in a selected ratio and preferably in particle size, and pharmaceutically and / or nutritionally acceptable excipients such as carriers, solubility enhancers, bioavailability enhancers, antioxidants, and optional flavorings, said composition exhibiting enhanced bioavailability. The lutein composition comprises at least 80% total lutein, wherein the total lutein comprises at least 65% by weight of trans-R,R lutein and at least 10% by weight of trans-R,R zeaxanthin, and is prepared by combining marigold and red pepper oleoresin in a ratio to produce a preferred ratio of trans-R,R lutein to trans-R,R zeaxanthin.

[0008] Therefore, the development of a lutein ester composition with excellent antioxidant and blue light damage resistance, which contains a high content of lutein ester microcapsule powder that is not easily degraded, is a research focus in this field. Summary of the Invention

[0009] In view of the shortcomings of the prior art, the object of the present invention is to provide a highly active composition for resisting blue light damage and a preparation method thereof.

[0010] In order to achieve the purpose of the invention, the present invention adopts the following technical solutions:

[0011] In a first aspect, the present invention provides a highly active composition for protecting against blue light damage, the composition comprising lutein ester and zeaxanthin;

[0012] The mass ratio of the lutein ester to zeaxanthin is 1:(0.8-1.5);

[0013] The lutein ester is added in the form of lutein ester microcapsule powder;

[0014] The raw materials of the lutein ester microcapsule powder do not contain other oil components except lutein ester crystals.

[0015] Preferably, the composition further comprises perilla seed oil.

[0016] Preferably, the mass ratio of the lutein ester, zeaxanthin and perilla seed oil is 1:(0.8-1.5):(0.1-1), for example, it can be 1:0.9:0.2, 1:0.9:0.4, 1:0.9:0.6, 1:0.9:0.8, 1:1:0.2, 1:1:0.4, 1:1:0.6, 1:1:0.8, 1:1.2:0.2, 1:1.2:0.4, 1:1.2:0.6, 1:1.2:0.8, 1:1.4:0.2, 1:1.4:0.4, 1:1.4:0.6, 1:1.4:0.8, etc.

[0017] The present invention combines lutein esters with zeaxanthin to create a composition with excellent antioxidant and blue light damage protection. The lutein ester microcapsule powder used in the present invention contains no oil components other than the lutein ester crystals, resulting in excellent stability and resistance to degradation. Furthermore, the addition of perilla seed oil to the composition synergistically enhances the composition's antioxidant and blue light damage protection.

[0018] Preferably, the raw materials of the lutein ester microcapsule powder include lutein ester crystals, emulsifier a, emulsifier b, fat-soluble antioxidant, water-soluble antioxidant, carrier and filling material.

[0019] Preferably, the raw materials of the lutein ester microcapsule powder include 12.5-32 parts of lutein ester crystals (for example, 13 parts, 15 parts, 17 parts, 19 parts, 21 parts, 23 parts, 25 parts, 27 parts, 29 parts, 31 parts, etc.), 1.5-2 parts of emulsifier a (for example, 1.6 parts, 1.7 parts, 1.8 parts, 1.9 parts, etc.), and emulsifier b. 1.5-2 parts (for example, 1.6 parts, 1.7 parts, 1.8 parts, 1.9 parts, etc.), 0.001-0.003 parts of fat-soluble antioxidants (for example, 0.0015 parts, 0.002 parts, 0.0025 parts, etc.), 2-4 parts of water-soluble antioxidants (for example, 2.5 parts, 3 parts, 3.5 parts, etc.), 35-50 parts of carriers (for example, 36 parts, 38 parts, 40 parts, 42 parts, 44 parts, 46 parts, 48 ​​parts, etc.) and 15-30 parts of filling materials (for example, 16 parts, 18 parts, 20 parts, 22 parts, 24 parts, 26 parts, 28 parts, etc.).

[0020] Preferably, emulsifier a includes emulsifiers with HLB values ​​of 12-15 and 15-18, wherein the HLB value of 12-15 may be, for example, 12.5, 13, 13.5, 14, 14.5, etc., and the HLB value of 15-18 may be, for example, 15.5, 16, 16.5, 17, 17.5, etc.

[0021] Preferably, the emulsifier b includes emulsifiers with HLB values ​​of 5-7 and 8-10. The HLB value of 5-7 may be, for example, 5.5, 6, 6.5, etc., and the HLB value of 8-10 may be, for example, 8.5, 9, 9.5, etc.

[0022] Preferably, the content of lutein ester in the lutein ester microcapsule powder is 10-25.5%, for example, it can be 11%, 12%, 13%, 14%, 15%, 16%, 17%, 18%, 19%, 20%, 21%, 22%, 23%, 24%, 25%, etc.

[0023] Preferably, the mass ratio of the emulsifiers with HLB values ​​of 12-15 and 15-18 in the emulsifier a is 1:(0.8-1.2), for example, it can be 1:0.9, 1:1, 1:1.1, etc.

[0024] Preferably, the mass ratio of the emulsifiers with HLB values ​​of 5-7 and 8-10 in the emulsifier b is 1:(0.8-1.2), for example, it can be 1:0.9, 1:1, 1:1.1, etc.

[0025] Other specific point values ​​within the above numerical ranges can be selected and will not be described in detail here.

[0026] Preferably, the emulsifier a and the emulsifier b are each independently selected from any one or a combination of at least two of sucrose fatty acid esters, monoglycerol fatty acid esters, diglycerol fatty acid esters, Tween or sorbitan monofatty acid esters.

[0027] Preferably, the fat-soluble antioxidant comprises ascorbyl palmitate.

[0028] Preferably, the water-soluble antioxidant comprises sodium ascorbate.

[0029] Preferably, the carrier comprises modified starch and / or gum arabic.

[0030] Preferably, the filling material comprises any one of sucrose, glucose, glucose syrup, isomaltooligosaccharide, fructooligosaccharide, solid corn syrup, xylitol, erythritol, resistant dextrin or fructooligosaccharide, or a combination of at least two thereof.

[0031] Preferably, the lutein ester microcapsule powder is prepared by the following method, which comprises:

[0032] (1) performing a first co-emulsification treatment on lutein ester crystals, a fat-soluble antioxidant, an emulsifier a, and a carrier to obtain a first co-emulsification product;

[0033] (2) The first co-emulsion obtained in step (1), the filler, the water-soluble antioxidant, the emulsifier b and water are subjected to a second co-emulsification treatment to obtain a second co-emulsion, which is then dried to obtain the lutein ester microcapsule powder.

[0034] Preferably, the first co-emulsification treatment and the second co-emulsification treatment each independently include any one of comminution, shearing or grinding.

[0035] Preferably, the temperature of the first co-emulsification treatment is -25 to -20°C (for example, -24°C, -23°C, -22°C, -21°C, etc.), the vacuum degree is 0.008-0.012 MPa (for example, 0.009 MPa, 0.01 MPa, 0.011 MPa, etc.), and the emulsification time is 15-30 min, for example, 16 min, 18 min, 20 min, 22 min, 24 min, 26 min, 28 min, etc.

[0036] Preferably, the particle size of the first co-emulsion is 10-30 μm, for example, 12 μm, 15 μm, 20 μm, 25 μm, 28 μm, etc.

[0037] Preferably, the temperature of the second co-emulsification treatment is 5-15°C (for example, 6°C, 8°C, 10°C, 12°C, 14°C, etc.), the vacuum degree is 0.035-0.045MPa (for example, 0.038MPa, 0.04MPa, 0.042MPa, etc.), and the emulsification time is 15-30min, for example, 16min, 18min, 20min, 22min, 24min, 26min, 28min, etc.

[0038] Preferably, the particle size of the second co-emulsion is less than 1 μm, for example, it may be 0.9 μm, 0.8 μm, 0.7 μm, 0.6 μm, 0.5 μm, 0.4 μm, 0.3 μm, 0.2 μm, 0.1 μm, 0.05 μm, etc.

[0039] The present invention is in a vacuum state during both the first co-emulsification process and the second co-emulsification process, which can effectively control the residual gas in the system and achieve the effect of reducing the amount of foam.

[0040] In the present invention, the addition of emulsifier a (hydrophilic emulsifier) ​​during the first co-emulsification process can effectively change the interfacial tension of the first co-emulsification, making it easier for the co-emulsion to merge with the water phase, which is beneficial for subsequent emulsification; the addition of emulsifier b (lipophilic emulsifier) ​​during the second co-emulsification process can effectively reduce the surface tension of water, thereby increasing the mutual attraction between water-soluble molecules and fat-soluble molecules and achieving interfacial equilibrium.

[0041] Other specific point values ​​within the above numerical ranges can be selected and will not be described here one by one

[0042] In a second aspect, the present invention provides a method for preparing a composition with high activity for resisting blue light damage as described in the first aspect, the preparation method comprising: uniformly mixing three raw materials, lutein ester, zeaxanthin and perilla seed oil, in the form of microcapsule powder.

[0043] Preferably, the preparation method comprises: uniformly mixing lutein ester microcapsule powder, zeaxanthin microcapsule powder and perilla seed oil microcapsule powder.

[0044] Preferably, the preparation method comprises:

[0045] (1) performing a first co-emulsification treatment on lutein ester, zeaxanthin, perilla seed oil, a fat-soluble antioxidant, an emulsifier a, and a carrier to obtain a first co-emulsification product;

[0046] (2) The first co-emulsion obtained in step (1), the filler material, the water-soluble antioxidant, the emulsifier b and water are subjected to a second co-emulsification treatment to obtain a second co-emulsion, which is then dried to obtain the highly active composition for resisting blue light damage.

[0047] Preferably, the preparation method comprises: uniformly mixing lutein ester microcapsule powder, zeaxanthin microcapsule powder and perilla seed oil microcapsule powder.

[0048] In the present invention, the zeaxanthin used contains two isomers, (3R, 3'R) zeaxanthin and (3R, 3'S) zeaxanthin, and the weight ratio of these two isomers in the zeaxanthin crystals is ≥80%; and the weight ratio between the two isomers, (3R, 3'R) zeaxanthin and (3R, 3'S) zeaxanthin, is (5-15):(95-85).

[0049] Compared with the prior art, the present invention has the following beneficial effects:

[0050] 1. The present invention combines lutein esters and zeaxanthin to obtain a composition with good antioxidant and blue light damage resistance effects. Furthermore, lutein esters, zeaxanthin and perilla seed oil are combined in a specific proportion to synergistically promote the antioxidant and blue light damage resistance effects of the composition. In the oxidative damage cell experiment, the cell survival rate of the composition provided by the present invention reached 98.38%.

[0051] 2. The raw material lutein ester microcapsule powder used in the present invention does not require high-temperature processing during the preparation process, which solves the instability problem caused by high-temperature melting of lutein ester during the preparation process and effectively avoids the problems of high-temperature sterilization instability or floating precipitation of lutein ester microcapsule powder during use. In addition, the lutein ester content in the lutein ester microcapsule powder can reach 10-25.5%. DETAILED DESCRIPTION

[0052] The technical solution of the present invention is further described below by way of specific embodiments. It should be understood by those skilled in the art that the embodiments are merely to help understand the present invention and should not be regarded as specific limitations of the present invention.

[0053] As used herein, the terms "comprises," "including," "having," "containing" or any other variations thereof, are intended to cover a non-exclusive inclusion. For example, a composition, process, method, article, or apparatus that comprises a listed element is not necessarily limited to only those elements but may include other elements not expressly listed or inherent to such composition, process, method, article, or apparatus.

[0054] "Optional" or "either" means that the subsequently described event or circumstance can or cannot occur, and that the description includes instances where the event occurs and instances where it does not.

[0055] The indefinite articles "a" and "an" before the elements or components of the present invention do not limit the quantity requirement (i.e. the number of times they appear). Therefore, "a" or "an" should be interpreted as including one or at least one, and elements or components in the singular also include plural forms, unless the quantity clearly refers to only the singular form.

[0056] The terms "one embodiment," "some embodiments," "exemplarily," "specific examples," or "some examples" used in the present invention mean that a specific feature, structure, material, or characteristic described in conjunction with the embodiment or example is included in at least one embodiment or example of the present invention. In this document, the exemplary expressions of the above terms do not necessarily refer to the same embodiment or example.

[0057] The sources of reagents or instruments in the following examples are as follows:

[0058] Zeaxanthin microcapsule powder: provided by Dalian Yinuo Biological Co., Ltd., containing 5% zeaxanthin, and the weight ratio of the two isomers of zeaxanthin, (3R, 3'R) zeaxanthin and (3R, 3'S) zeaxanthin, is (5-15): (95-85);

[0059] Zeaxanthin crystals: provided by Dalian Yinuo Biological Co., Ltd., containing 72% zeaxanthin;

[0060] Perilla seed oil microcapsule powder: purchased from Dalian Yinuo Biological Co., Ltd., containing 50% perilla seed oil;

[0061] Lutein ester crystals: total pigment content is 86%, trans-lutein liquid phase content is 93%, and water content is 3%;

[0062] Other raw materials used in the preparation examples, comparative preparation examples, embodiments, comparative examples or application examples of the present invention are conventional commercially available products;

[0063] It should be noted that the fat-soluble antioxidants in the raw materials of the lutein ester microcapsule powder in the following preparation examples and comparative preparation examples are measured by content (unit: ppm) due to their small amount, and other raw materials are measured by parts by weight.

[0064] Preparation Example 1

[0065] This preparation example provides a lutein ester microcapsule powder, the raw materials of which include:

[0066] Lutein ester crystals 20 parts, emulsifier a 2 parts, emulsifier b 2 parts, VC palmitate 20ppm, VC sodium 3 parts, modified starch 48 parts, xylitol 25 parts;

[0067] Emulsifier a includes: 1 part of Tween with an HLB value of 12-15 and 1 part of Tween with an HLB value of 15-18;

[0068] Emulsifier b includes: 1 part of Tween with an HLB value of 5-7 and 1 part of Tween with an HLB value of 8-10;

[0069] The preparation method of the lutein ester microcapsule powder is as follows:

[0070] (1) mixing lutein ester crystals, VC palmitate, emulsifier a, and modified starch, and subjecting them to a shear emulsification treatment at -23°C and a vacuum degree of 0.01 MPa for 20 minutes to obtain a first co-emulsion;

[0071] (2) The first co-emulsion obtained in step (1), xylitol, sodium VC, emulsifier b and 150 parts of water were mixed, and shear emulsification treatment was performed at 10° C. and a vacuum degree of 0.04 MPa for 20 minutes to obtain a second co-emulsion, and the second co-emulsion was spray-dried to obtain the lutein ester microcapsule powder.

[0072] Preparation Example 2

[0073] This preparation example provides a lutein ester microcapsule powder, the raw materials of which include:

[0074] Lutein ester crystals 12.5 parts, emulsifier a 1.6 parts, emulsifier b 2 parts, VC palmitate 10ppm, VC sodium 4 parts, gum arabic 49.5 parts, glucose 30 parts;

[0075] Emulsifier a includes: 0.8 parts of sucrose fatty acid ester with an HLB value of 12-15, and 0.8 parts of sucrose fatty acid ester with an HLB value of 15-18;

[0076] Emulsifier b includes: 1 part of sucrose fatty acid ester with an HLB value of 5-7, and 1 part of sucrose fatty acid ester with an HLB value of 8-10;

[0077] The preparation method of the lutein ester microcapsule powder is as follows:

[0078] (1) mixing lutein ester crystals, VC palmitate, emulsifier a, and gum arabic, and subjecting them to a shear emulsification treatment at -20°C and a vacuum degree of 0.01 MPa for 30 minutes to obtain a first co-emulsion;

[0079] (2) The first co-emulsion obtained in step (1), glucose, sodium VC, emulsifier b and 150 parts of water were mixed, and shear emulsification treatment was performed at 15° C. and a vacuum degree of 0.04 MPa for 15 minutes to obtain a second co-emulsion, and the second co-emulsion was spray-dried to obtain the lutein ester microcapsule powder.

[0080] Preparation Example 3

[0081] This preparation example provides a lutein ester microcapsule powder, the raw materials of which include:

[0082] 32 parts of lutein ester crystals, 2 parts of emulsifier a, 1.6 parts of emulsifier b, 30 ppm of VC palmitate, 2 parts of VC sodium, 42.4 parts of modified starch, 20 parts of isomaltooligosaccharide;

[0083] Emulsifier a includes: 1 part of Tween with an HLB value of 12-15 and 1 part of Tween with an HLB value of 15-18;

[0084] Emulsifier b includes: 0.8 parts of Tween with an HLB value of 5-7 and 0.8 parts of Tween with an HLB value of 8-10;

[0085] The preparation method of the lutein ester microcapsule powder is as follows:

[0086] (1) mixing lutein ester crystals, VC palmitate, emulsifier a, and modified starch, and subjecting them to a shear emulsification treatment at -25°C and a vacuum degree of 0.01 MPa for 15 minutes to obtain a first co-emulsion;

[0087] (2) The first co-emulsion obtained in step (1), isomaltooligosaccharide, sodium VC, emulsifier b and 150 parts of water were mixed, and shear emulsification treatment was performed at 5° C. and a vacuum degree of 0.04 MPa for 30 minutes to obtain a second co-emulsion, and the second co-emulsion was spray-dried to obtain the lutein ester microcapsule powder.

[0088] Preparation Example 4

[0089] This preparation example provides a lutein ester microcapsule powder, which differs from Preparation Example 1 only in the emulsifier a. The emulsifier a in this preparation example includes: 1.2 parts of Tween with an HLB value of 12-15 and 0.8 parts of Tween with an HLB value of 15-18; other raw materials, amounts and preparation methods are the same as those in Preparation Example 1.

[0090] Preparation Example 5

[0091] This preparation example provides a lutein ester microcapsule powder, which differs from Preparation Example 1 only in the emulsifier a. The emulsifier a in this preparation example includes: 0.8 parts of Tween with an HLB value of 12-15 and 1.2 parts of Tween with an HLB value of 15-18; other raw materials, amounts and preparation methods are the same as those in Preparation Example 1.

[0092] Preparation Example 6

[0093] This preparation example provides a lutein ester microcapsule powder, which differs from Preparation Example 1 only in the emulsifier b. The emulsifier b in this preparation example includes: 1.2 parts of Tween with an HLB value of 5-7 and 0.8 parts of Tween with an HLB value of 8-10; other raw materials, amounts and preparation methods are the same as those in Preparation Example 1.

[0094] Preparation Example 7

[0095] This preparation example provides a lutein ester microcapsule powder, which differs from Preparation Example 1 only in the emulsifier b. The emulsifier b in this preparation example includes: 0.8 parts of Tween with an HLB value of 5-7 and 1.2 parts of Tween with an HLB value of 8-10; other raw materials, amounts and preparation methods are the same as those in Preparation Example 1.

[0096] Preparation Example 8

[0097] This preparation example provides a lutein ester microcapsule powder, which differs from Preparation Example 1 only in that VC palmitate is replaced by an equal amount of VE (vitamin E); other raw materials, amounts and preparation methods are the same as those in Preparation Example 1.

[0098] Preparation Example 9

[0099] This preparation example provides a lutein ester microcapsule powder, which differs from Preparation Example 1 only in that sodium VC is replaced with an equal amount of VC (vitamin C); other raw materials, amounts and preparation methods are the same as those in Preparation Example 1.

[0100] Comparative Preparation Example 1

[0101] This comparative preparation example provides a lutein ester microcapsule powder, which differs from Example 1 only in that Tween with an HLB value of 15-18 is not added to the emulsifier a. The total amount of emulsifier a remains unchanged, and the insufficient amount is supplemented by Tween with an HLB value of 12-15. Other raw materials, amounts, and preparation methods are the same as those in Example 1.

[0102] Comparative Preparation Example 2

[0103] This comparative preparation example provides a lutein ester microcapsule powder, which differs from Example 1 only in that Tween with an HLB value of 12-15 is not added to the emulsifier a. The total amount of emulsifier a remains unchanged, and the insufficient amount is supplemented by Tween with an HLB value of 15-18. Other raw materials, amounts, and preparation methods are the same as those in Example 1.

[0104] Comparative Preparation Example 3

[0105] This comparative preparation example provides a lutein ester microcapsule powder, which differs from Example 1 only in that Tween with an HLB value of 8-10 is not added to the emulsifier b. The total amount of emulsifier b remains unchanged, and the insufficient amount is supplemented by Tween with an HLB value of 5-7. Other raw materials, amounts, and preparation methods are the same as those in Example 1.

[0106] Comparative Preparation Example 4

[0107] This comparative preparation example provides a lutein ester microcapsule powder, which differs from Example 1 only in that Tween with an HLB value of 5-7 is not added to the emulsifier b. The total amount of emulsifier b remains unchanged, and the insufficient amount is supplemented by Tween with an HLB value of 8-10. Other raw materials, amounts, and preparation methods are the same as those in Example 1.

[0108] Comparative Preparation Example 5

[0109] This comparative preparation example provides a lutein ester microcapsule powder, which differs from Example 1 only in the preparation method. The preparation method of this comparative preparation example is as follows:

[0110] (1) Lutein ester crystals, VC palmitate, emulsifier a, modified starch, xylitol, VC sodium, emulsifier b and 150 parts of water are mixed uniformly, and shear emulsification treatment is performed at 10° C. and a vacuum degree of 0.04 MPa for 20 minutes to obtain a co-emulsion, and the co-emulsion is spray-dried to obtain the lutein ester microcapsule powder.

[0111] Comparative Preparation Example 6

[0112] This comparative preparation example provides a lutein ester microcapsule powder, which differs from Example 1 only in the preparation method. The preparation method of this comparative example is as follows:

[0113] Refer to the method of Example 1 in CN112869155A:

[0114] Raw material composition: lutein ester crystals 25g, molecular distilled monoglyceride 112.5g, sodium starch octenylsuccinate 150g, maltodextrin 115g, sucrose 60g, L-ascorbic acid 12.5g, vitamin E 25g.

[0115] Preparation method:

[0116] (1) dissolving the above-mentioned weight amounts of sodium starch octenylsuccinate, maltodextrin, sucrose, and L-ascorbic acid in pure water at 70° C. to prepare an aqueous phase;

[0117] (2) melting the lutein ester in molecularly distilled monoglyceride with added vitamin E at 70°C to obtain an oil phase;

[0118] (3) Add the oil phase to the water phase under high shear emulsification conditions at 7000 r / min, and continue emulsification for 10 min after the addition is completed to obtain a primary emulsion;

[0119] (4) The primary emulsion was first ground with 0.4-0.6 mm zirconia balls to a particle size of 0.25 μm, and then replaced with 0.2-0.4 mm zirconia balls to continue grinding the liquid to a particle size of 0.08 μm.

[0120] (5) The ground emulsion is spray-dried to obtain the product.

[0121] Test Example 1

[0122] According to the Chinese Pharmacopoeia accelerated stability evaluation method, pigment content was measured at different times under conditions of 40°C and 75% RH to determine product stability. Pigment retention was used to indicate product stability. Pigment retention is the ratio of the product content at different times to the initial content, expressed as a percentage. "Slight oily speckling" indicates ≤5% surface oily speckling; "Oil scattering +" indicates 10-25% surface oily speckling; "Oil scattering ++" indicates 25-40% surface oily speckling; "Oil scattering +++" indicates 40-60% surface oily speckling; and "Oil scattering" indicates visible oil droplets or layers. The results are shown in Table 1.

[0123] Table 1

[0124]

[0125]

[0126] According to the data in the table, when the emulsifier a and emulsifier b provided by the present invention are used, the content of lutein ester in the microcapsule powder is the highest and the stability of the microcapsule powder is the best. When the proportion of emulsifiers with an HLB value of 12-15 in emulsifier a is too high or too low, the emulsification effect is poor and no bridging effect is achieved. When the proportion of emulsifiers with an HLB value of 5-7 in emulsifier b is too high, there are too many lipophilic emulsifiers, which affects the water-oil balance. When the proportion is too low, it is insufficient to provide an emulsifier with a low HLB value, and the oil phase emulsification effect deteriorates. When VE is used as a fat-soluble antioxidant, the antioxidant capacity of the oil phase becomes weak, the product stability deteriorates, and VE is not It is conducive to emulsification, resulting in an increase in particle size and lower stability. When VC is used as a water-soluble antioxidant, the pH of the aqueous phase changes, and it cannot form a buffer ion pair with citric acid during sterilization at 90 degrees like sodium VC, so it also has an adverse effect on stability. When emulsifier a uses a single emulsifier with an HLB value of 15-18 or an emulsifier with an HLB value of 12-15, a good emulsification system is not formed, resulting in insufficient hydrophilicity of the first co-emulsion. When emulsifier b uses a single emulsifier with an HLB value of 8-10 or an emulsifier with an HLB value of 5-7, the oil phase affinity is insufficient or the link with the aqueous phase emulsifier is insufficient.

[0127] In addition, in Comparative Preparation Example 6, lutein ester microcapsule powder was prepared with reference to CN112869155A. The theoretical content of the obtained microcapsule powder was 5.0%, while the actual measured content was 4.1%, indicating that there was lutein ester processing loss during the high-temperature preparation process, with a loss rate of 18%. That is, during the high-temperature processing process, 18% of the lutein ester was lost due to the high temperature.

[0128] Example 1

[0129] This embodiment provides a highly active composition for protecting against blue light damage, wherein the raw materials of the composition include: 6.25 parts of lutein ester microcapsule powder prepared in Preparation Example 1, 20 parts of zeaxanthin microcapsule powder, and 1 part of perilla seed oil microcapsule powder;

[0130] The aforementioned raw materials were mixed according to the formula amounts to obtain the highly active composition for protecting against blue light damage (the mass ratio of lutein ester, zeaxanthin and perilla seed oil in the composition was 1:1:0.5).

[0131] Example 2

[0132] This embodiment provides a highly active composition for protecting against blue light damage, wherein the raw materials of the composition include: 6.25 parts of lutein ester microcapsule powder prepared in Preparation Example 1, 16 parts of zeaxanthin microcapsule powder, and 2 parts of perilla seed oil microcapsule powder;

[0133] The aforementioned raw materials were mixed according to the formula amounts to obtain the highly active composition for protecting against blue light damage (the mass ratio of lutein ester, zeaxanthin and perilla seed oil in the composition was 1:0.8:1).

[0134] Example 3

[0135] This embodiment provides a highly active composition for protecting against blue light damage, wherein the raw materials of the composition include: 6.25 parts of lutein ester microcapsule powder prepared in Preparation Example 1, 30 parts of zeaxanthin microcapsule powder, and 0.2 parts of perilla seed oil microcapsule powder;

[0136] The aforementioned raw materials were mixed according to the formula amounts to obtain the highly active composition for protecting against blue light damage (the mass ratio of lutein ester, zeaxanthin and perilla seed oil in the composition was 1:1.5:0.1).

[0137] Example 4

[0138] This preparation example provides a highly active composition for protecting against blue light damage. The raw materials of the microcapsule powder include:

[0139] 8 parts of lutein ester crystals, 9 parts of zeaxanthin crystals, 3.2 parts of perilla seed oil, 2 parts of emulsifier a, 2 parts of emulsifier b, 20 ppm of VC palmitate, 3 parts of VC sodium, 48 parts of modified starch, and 25 parts of xylitol;

[0140] Emulsifier a includes: 1 part of Tween with an HLB value of 12-15 and 1 part of Tween with an HLB value of 15-18;

[0141] Emulsifier b includes: 1 part of Tween with an HLB value of 5-7 and 1 part of Tween with an HLB value of 8-10;

[0142] The preparation method of the highly active composition for resisting blue light damage is as follows:

[0143] (1) mixing lutein ester crystals, zeaxanthin crystals, perilla seed oil, VC palmitate, emulsifier a, and modified starch, and subjecting the mixture to a shear emulsification treatment at -23°C and a vacuum degree of 0.01 MPa for 20 minutes to obtain a first co-emulsion;

[0144] (2) The first co-emulsion obtained in step (1), xylitol, sodium VC, emulsifier b, and 150 parts of water were mixed and subjected to shear emulsification treatment at 10° C. and a vacuum degree of 0.04 MPa for 20 minutes to obtain a second co-emulsion. The second co-emulsion was spray-dried to obtain the highly active composition for protecting against blue light damage. (The mass ratio of lutein ester, zeaxanthin, and perilla seed oil in the composition is 1:1:0.5)

[0145] Example 5

[0146] This embodiment provides a highly active composition for protecting against blue light damage, wherein the raw materials of the composition include: 6.25 parts of lutein ester microcapsule powder prepared in Preparation Example 1 and 20 parts of zeaxanthin microcapsule powder;

[0147] The aforementioned raw materials are mixed according to the formula amounts to obtain the highly active composition for protecting against blue light damage (the mass ratio of lutein ester to zeaxanthin in the composition is 1:1).

[0148] Example 6

[0149] This preparation example provides a highly active composition for protecting against blue light damage. The raw materials of the microcapsule powder include:

[0150] 8 parts of lutein ester crystals, 9 parts of zeaxanthin crystals, 2 parts of emulsifier a, 2 parts of emulsifier b, 20 ppm of VC palmitate, 3 parts of VC sodium, 48 parts of modified starch, and 25 parts of xylitol;

[0151] Emulsifier a includes: 1 part of Tween with an HLB value of 12-15 and 1 part of Tween with an HLB value of 15-18;

[0152] Emulsifier b includes: 1 part of Tween with an HLB value of 5-7 and 1 part of Tween with an HLB value of 8-10;

[0153] The preparation method of the highly active composition for resisting blue light damage is as follows:

[0154] (1) mixing lutein ester crystals, zeaxanthin crystals, VC palmitate, emulsifier a, and modified starch, and subjecting the mixture to a shear emulsification treatment at -23°C and a vacuum degree of 0.01 MPa for 20 minutes to obtain a first co-emulsion;

[0155] (2) The first co-emulsion obtained in step (1), xylitol, sodium VC, emulsifier b, and 150 parts of water were mixed and subjected to shear emulsification treatment at 10° C. and a vacuum degree of 0.04 MPa for 20 minutes to obtain a second co-emulsion. The second co-emulsion was spray-dried to obtain the highly active composition for protecting against blue light damage. (The mass ratio of lutein ester to zeaxanthin in the composition is 1:1)

[0156] Comparative Example 1

[0157] This comparative example provides a highly active composition for protecting against blue light damage, wherein the raw materials of the composition include 9.37 parts of lutein ester microcapsule powder prepared in Preparation Example 1, 20 parts of zeaxanthin microcapsule powder, and 1 part of perilla seed oil microcapsule powder;

[0158] The aforementioned raw materials were mixed according to the formula amounts to obtain the highly active composition for protecting against blue light damage (the mass ratio of lutein ester, zeaxanthin and perilla seed oil in the composition was 1.5:1:0.5).

[0159] Comparative Example 2

[0160] This comparative example provides a highly active composition for protecting against blue light damage, the raw materials of the composition comprising: 6.25 parts of lutein ester microcapsule powder prepared in Preparation Example 1, 36 parts of zeaxanthin microcapsule powder, and 1 part of perilla seed oil microcapsule powder;

[0161] The aforementioned raw materials were mixed according to the formula amounts to obtain the highly active composition for protecting against blue light damage (the mass ratio of lutein ester, zeaxanthin and perilla seed oil in the composition was 1:1.8:0.5).

[0162] Comparative Example 3

[0163] This comparative example provides a highly active composition for protecting against blue light damage, the raw materials of the composition comprising: 6.25 parts of lutein ester microcapsule powder prepared in Preparation Example 1, 20 parts of zeaxanthin microcapsule powder, and 2.6 parts of perilla seed oil microcapsule powder;

[0164] The aforementioned raw materials were mixed according to the formula amounts to obtain the highly active composition for protecting against blue light damage (the mass ratio of lutein ester, zeaxanthin and perilla seed oil in the composition was 1:1:1.3).

[0165] Comparative Example 4

[0166] This comparative example provides a highly active composition for protecting against blue light damage, wherein the raw materials of the composition include: 6.25 parts of lutein ester microcapsule powder prepared in Preparation Example 1 and 1 part of perilla seed oil microcapsule powder;

[0167] The aforementioned raw materials were mixed according to the formula amounts to obtain the highly active composition for resisting blue light damage (the mass ratio of lutein ester to perilla seed oil in the composition was 1:0.5).

[0168] Comparative Example 5

[0169] This comparative example provides a highly active composition for protecting against blue light damage, wherein the raw materials of the composition include: 20 parts of zeaxanthin microcapsule powder and 1 part of perilla seed oil microcapsule powder;

[0170] The aforementioned raw materials were mixed according to the formula amounts to obtain the highly active composition for resisting blue light damage (the mass ratio of zeaxanthin to perilla seed oil in the composition was 1:0.5).

[0171] Comparative Example 6

[0172] This comparative example provides a highly active composition for protecting against blue light damage, wherein the raw materials of the composition include: 6.25 parts of lutein ester and 10 parts of zeaxanthin;

[0173] The aforementioned raw materials were mixed according to the formula amounts to obtain the highly active composition for protecting against blue light damage (the mass ratio of lutein ester to zeaxanthin in the composition was 1:0.5).

[0174] Test Example 2

[0175] Oxidative damage test-cell experiment

[0176] Experimental process:

[0177] ARPE-19 ocular cells in logarithmic growth phase were cultured at 1×10 4 Each well was evenly inoculated into a 96-well culture plate and cultured for 24 h as a blank control group;

[0178] Hydrogen peroxide group: ARPE-19 ocular cells in the logarithmic growth phase were cultured at a concentration of 1×10 4 Cells were evenly seeded into 96-well culture plates, cultured for 24 h, and then treated with hydrogen peroxide (500 μM) for 2 h to induce oxidative damage.

[0179] Treatment group: ARPE-19 ocular cells in the logarithmic growth phase were injected at a rate of 1×10 4 The cells / well were evenly seeded into a 96-well culture plate and cultured for 24 h. 20 μM of the highly active composition for protecting against blue light damage prepared in the examples and comparative examples was added and treated for 24 h. Subsequently, hydrogen peroxide (500 μM) was used to induce oxidative damage for 2 h.

[0180] The above three groups used CCK-8 kit to measure the survival rate of cells in each group using a microplate reader to reflect the antioxidant level.

[0181] Result analysis: Cell viability (%) = (absorbance of experimental group - absorbance of blank group) / (absorbance of control group - absorbance of blank group) × 100%. The results are shown in Table 2.

[0182] Table 2

[0183]

[0184]

[0185] As can be seen from the table, the compositions of Examples 1-3 have good antioxidant activity and can significantly improve the survival rate of ocular cells after hydrogen peroxide damage; as can be seen from Example 1 and Comparative Examples 1-6, when any one of the three raw materials of lutein ester, zeaxanthin and perilla seed oil in the composition is excessive or insufficient, the improvement in the survival ability of ARPE-19 ocular cells is reduced; when any one of the three raw materials of lutein ester, zeaxanthin and perilla seed oil in the composition is lacking, the cell survival rate after oxidative damage is reduced, indicating that the three raw materials act synergistically to jointly promote the antioxidant properties of the composition.

[0186] Test Example 3

[0187] Anti-blue light damage test-animal experiment

[0188] Experimental animals:

[0189] Kunming mice (KM), male, average weight 33 g, were purchased from Liaoning Changsheng Biotechnology Co., Ltd. Mice were housed for 4–6 weeks with 12 h of light daily and adequate water and food. All animal experiments were approved by the Dalian Medical University Animal Care and Use Committee (Ethics Number: AEE21112).

[0190] Drugs and reagents:

[0191] Malondialdehyde (MDA) kit, total superoxide dismutase (T-SOD) kit, and glutathione peroxidase (GSH-PX) kit were purchased from Nanjing Jiancheng Bioengineering Institute.

[0192] Experimental methods:

[0193] Establishment of the blue light damage model in mice and administration of the composition with high resistance to blue light damage. According to the experimental grouping design, the mice were divided into the following groups:

[0194] Blank group: physiological saline was administered for 14 consecutive days, and then dark conditions were maintained for 12 h after the end of administration;

[0195] Blue light group: Normal saline was administered for 14 consecutive days, and then irradiated with blue light with an average illumination of 4000-5333 Lux for 12 hours;

[0196] Experimental Group: Each mouse was administered 20 mg / kg of the test substance (converted to a lutein ester content of 20 mg / kg) daily for 14 consecutive days. After the end of the administration period, the mice were irradiated with blue light at an average illumination of 4000-5333 Lux for 12 hours. The test substances included: lutein ester crystals, lutein ester microcapsule powders obtained in Preparation Examples 1-3 and Comparative Preparation Example 6, and the compositions prepared in Examples 1-5.

[0197] After the blue light exposure, the mice were sacrificed, and serum (without hemolysis) and retinal tissue (stripped of nerves and blood vessels) were collected. Serum MDA, T-SOD, and GSH-PX levels were measured according to the MDA, T-SOD, and GSH-PX assay kits, respectively.

[0198] Result analysis: Based on the results of the blank group, calculate the content of all indicators in each group. The results are compared with the blue light group and presented as the increase / decrease multiples of the content.

[0199] The calculation formula is:

[0200] T-SOD growth factor = (experimental group / blue light group-1);

[0201] GSH-PX growth factor = (experimental group / blue light group-1);

[0202] MDA reduction factor = blue light group / experimental group - 1. The test results are shown in Table 3.

[0203] Table 3

[0204] sample MDA decline multiple T-SOD growth multiple GSH-PX growth multiple Lutein ester crystals 0.13 2.35 1.56 Preparation Example 1 0.44 4.20 1.85 Preparation Example 2 0.39 4.23 1.95 Preparation Example 3 0.41 4.18 1.96 Comparative Preparation Example 6 0.15 2.35 1.52 Example 1 32.2 6.1 2.2 Example 2 32.5 6.2 2.25 Example 3 32.3 6.0 2.32 Example 4 28.35 5.97 2.05 Example 5 28.14 5.95 2.01 Example 6 28.44 5.90 2.07

[0205] According to the data in the table, it can be seen that when the lutein ester microcapsule powder of Preparation Examples 1-3 provided by the present invention is directly used as the test substance, its MDA reduction multiple is more than 2.5 times that of the crystal group and the comparative preparation example 6, indicating that the lutein ester microcapsule powder provided by the present invention has a good effect of resisting blue light damage.

[0206] As can be seen from the data of Example 5, the MDA reduction factor of the composition obtained by compounding the lutein ester microcapsule powder prepared by the present invention with zeaxanthin microcapsule powder is more than 216 times that of the crystal group, and has excellent protection against blue light damage.

[0207] After the lutein ester microcapsule powder prepared by the present invention is compounded with zeaxanthin microcapsule powder and linseed oil microcapsule powder, the MDA reduction multiple of the composition is more than 245 times that of the crystal group, which shows that the composition provided by the present invention has excellent effect in resisting blue light damage.

[0208] The applicant declares that the present invention is illustrated by the above-described embodiments, but the present invention is not limited to these embodiments. This does not mean that the present invention must rely on these embodiments in order to be implemented. Those skilled in the art should understand that any improvements to the present invention, equivalent substitutions for raw materials in the present invention, additions of auxiliary ingredients, and selection of specific methods, etc., fall within the scope of protection and disclosure of the present invention.

[0209] The preferred embodiments of the present invention are described in detail above. However, the present invention is not limited to the specific details in the above embodiments. Within the technical concept of the present invention, various simple modifications can be made to the technical solution of the present invention, and these simple modifications all fall within the scope of protection of the present invention.

[0210] It should also be noted that the various specific technical features described in the above specific embodiments can be combined in any appropriate manner without contradiction. In order to avoid unnecessary repetition, the present invention will not further describe various possible combinations.

Claims

1. A composition for resisting blue light damage, characterized in that: The active ingredients of the composition are lutein esters, zeaxanthin and perilla seed oil; The mass ratio of the lutein ester, zeaxanthin and perilla seed oil is 1:(0.8-1.5):(0.1-1); The lutein ester is added in the form of lutein ester microcapsule powder; the content of lutein ester in the lutein ester microcapsule powder is 10-25.5%; The raw materials of the lutein ester microcapsule powder include lutein ester crystals, emulsifier a, emulsifier b, fat-soluble antioxidant, water-soluble antioxidant, carrier and filling material; The emulsifier a is a hydrophilic emulsifier, including emulsifiers with HLB values ​​of 12-15 and 15-18; the mass ratio of the emulsifiers with HLB values ​​of 12-15 and 15-18 in the emulsifier a is 1:(0.8-1.2); The emulsifier b is a lipophilic emulsifier, including emulsifiers with HLB values ​​of 5-7 and 8-10; the mass ratio of the emulsifiers with HLB values ​​of 5-7 and 8-10 in the emulsifier b is 1:(0.8-1.2); The raw materials of the lutein ester microcapsule powder do not contain any other oil components except lutein ester crystals; The lutein ester microcapsule powder is prepared by the following method, which comprises: (1) performing a first co-emulsification treatment on the lutein ester crystals, the fat-soluble antioxidant, the emulsifier a, and the carrier to obtain a first co-emulsification product; the temperature of the first co-emulsification treatment is -25 to -20°C, the vacuum degree is 0.008 to 0.012 MPa, and the emulsification time is 15 to 30 min; (2) The first co-emulsion obtained in step (1), the filler material, the water-soluble antioxidant, the emulsifier b and water are subjected to a second co-emulsification treatment to obtain a second co-emulsion, which is then dried to obtain the lutein ester microcapsule powder; the temperature of the second co-emulsification treatment is 5-15°C, the vacuum degree is 0.035-0.045 MPa, and the emulsification time is 15-30 min.

2. The composition for resisting blue light damage according to claim 1, characterized in that The emulsifier a and the emulsifier b are each independently selected from any one or a combination of at least two of sucrose fatty acid esters, monoglycerol fatty acid esters, diglycerol fatty acid esters, Tween or sorbitan monofatty acid esters.

3. The composition for resisting blue light damage according to claim 1, characterized in that The fat-soluble antioxidant includes ascorbyl palmitate.

4. The composition for resisting blue light damage according to claim 1, characterized in that The water-soluble antioxidant includes sodium ascorbate.

5. The composition for resisting blue light damage according to claim 1, characterized in that: The carrier includes modified starch and / or gum arabic.

6. The composition for resisting blue light damage according to claim 1, characterized in that The filling material includes any one of sucrose, glucose, glucose syrup, isomaltooligosaccharide, fructooligosaccharide, solid corn syrup, xylitol, erythritol, resistant dextrin or fructooligosaccharide, or a combination of at least two thereof.

7. The composition for resisting blue light damage according to claim 1, characterized in that: The particle size of the first co-emulsion is 10-30 μm.

8. The composition for protecting against blue light damage according to claim 1, characterized in that: The particle size of the second co-emulsion is less than 1 μm.

9. A method for preparing the composition for protecting against blue light damage according to any one of claims 1 to 8, characterized in that: The preparation method comprises the following steps: uniformly mixing three raw materials, lutein ester, zeaxanthin and perilla seed oil, in the form of microcapsule powder to obtain the product.

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