Lutein ester and zeaxanthin compound microcapsule, and preparation method and application thereof

Abstract

The present application provides a kind of lutein ester and zeaxanthin compound microcapsule and its preparation method and application, the lutein ester and zeaxanthin compound microcapsule includes the mass ratio of 10:1-5:1 lutein ester and zeaxanthin, also includes wall material, filling agent, compound emulsifier, oil-soluble antioxidant, vegetable oil and pure water, the compound emulsifier is the mass ratio of (4.2-5) :(1.5-2) :(2.6-3.5) glycerol monostearate, sorbitol anhydrous monostearate and sucrose fatty acid ester.The lutein ester and zeaxanthin compound microcapsule of the present application has the effect of protecting eyes, preventing eye diseases, relieving eye fatigue, improving eyesight, can also be further processed into functional food, can meet the demand of people to eye health.

Description

TECHNICAL FIELD

[0001] The present application relates to the technical field of functional foods, in particular to a lutein ester and zeaxanthin compound microcapsule, a preparation method and application thereof. BACKGROUND

[0002] Lutein ester and zeaxanthin are important nutrients for eye health, and they play an important role in protecting the eyes from ultraviolet damage, delaying eye aging, preventing eye diseases, etc. However, in daily life, people often lack enough nutrients due to unbalanced diet, fast-paced life, etc. Therefore, it is of great practical significance and market value to develop an eye care product containing lutein ester and zeaxanthin.

[0003] CN109123646A discloses a product containing zeaxanthin and lutein ester and a preparation method thereof, which directly mixes and presses zeaxanthin and lutein ester with other auxiliary materials into tablets, without considering the problem that the two polar substances are difficult to mix uniformly, so the product effect is not good.

[0004] In view of the above problems, the prior art such as CN116530680A, CN109938146A and CN116898050A first prepares lutein ester microcapsule powder, and then mixes it with zeaxanthin, other auxiliary materials to prepare eye care products of different dosage forms. However, there is still a risk of uneven mixing, and it is difficult to ensure that lutein ester and zeaxanthin are within the optimal eye care ratio range. SUMMARY

[0005] In view of the deficiencies of the prior art, the present application provides a lutein ester and zeaxanthin compound microcapsule, a preparation method and application thereof.

[0006] In a first aspect, the present application provides a lutein ester and zeaxanthin compound microcapsule, which comprises lutein ester and zeaxanthin in a mass ratio of 10:1-5:1, and further comprises wall material, filler, compound emulsifier, oil-soluble antioxidant, vegetable oil and pure water, wherein the compound emulsifier is glycerol monostearate, sorbitan monostearate and sucrose fatty acid ester in a mass ratio of (4.2-5):(1.5-2):(2.6-3.5).

[0007] When lutein ester and zeaxanthin are compounded in a mass ratio of 10:1-5:1 (mass ratio of pure substances), the proportion of lutein and zeaxanthin in the eyes of people is the same, and therefore good eye protection effects such as prevention of visual fatigue and prevention of cataract are achieved. However, if zeaxanthin and lutein ester are directly mixed and compounded into microcapsules by a conventional method for preparing lutein ester microcapsule powder, the obtained compounded microcapsules are prone to oil leakage, and if subsequent tabletting is performed, the obtained product is also prone to chipped tablets. In summary, the stability is poor. The present application has found that the use of a compounded emulsifier composed of a specific ratio of glycerol monostearate, sorbitan monostearate and sucrose fatty acid ester is conducive to the uniform mixing of zeaxanthin and lutein ester.

[0008] In some embodiments of the present application, the preparation method of the compounded emulsifier is as follows: glycerol monostearate, sorbitan monostearate and sucrose fatty acid ester are added to ethyl acetate, the mass ratio of the total mass of the three emulsifiers to the mass of ethyl acetate is 1:1, and heating and dissolution are performed at 50°C, followed by ultrasonic treatment for 20-25 min and concentration to a residual amount of ethyl acetate of ≤25 ppm.

[0009] In the above technical solution, the compounded emulsifier is premixed in advance, which is conducive to obtaining better emulsification effect subsequently.

[0010] In some embodiments of the present application, the lutein ester and zeaxanthin compounded microcapsule comprises the following components in parts by weight:

[0011] Lutein ester 4.5-5.5 parts, zeaxanthin 0.45-1.1 parts, wall material 18-26 parts, filler 14-23 parts, compounded emulsifier 1.2-1.45 parts, oil-soluble antioxidant 0.55-0.8 parts, vegetable oil 0.5-2 parts and pure water 38-55 parts. Among them, the parts by weight of lutein ester and zeaxanthin refer to pure weight parts. The purity of lutein ester and zeaxanthin purchased on the market generally does not reach 100%, and therefore it is necessary to convert it to ensure that the pure amount meets the formula requirements.

[0012] In some embodiments of the present application, the wall material is one or more of sodium alginate, gum arabic, modified starch and gelatin.

[0013] In some embodiments of the present application, the filler is one or more of sucrose, maltose, oligomeric isomaltose and malt dextrin.

[0014] In some embodiments of the present application, the oil-soluble antioxidant is any one of vitamin E and rosemary extract.

[0015] In some embodiments of the present application, the vegetable oil is one or more of grape seed oil, soybean oil, safflower seed oil and medium-chain triglyceride.

[0016] The lutein ester and zeaxanthin compound microcapsule provided by the present application contains lutein ester ≥10% and zeaxanthin ≥1%, and the particle size of the microcapsule is between 40-100 mesh.

[0017] In a second aspect, the present application provides a preparation method of the lutein ester and zeaxanthin compound microcapsule.

[0018] The preparation method provided by the present application comprises the following steps:

[0019] (1) adding wall material, filler, compound emulsifier and zeaxanthin into pure water, heating and stirring to dissolve, and nano-grinding to obtain an aqueous phase;

[0020] (2) melting lutein ester in a mixture of vegetable oil and oil-soluble antioxidant to obtain an oil phase;

[0021] (3) adding the oil phase into the high-speed sheared aqueous phase to emulsify, then homogenizing, grinding the homogenized emulsion to obtain a ground emulsion;

[0022] (4) performing one-step granulation on the ground emulsion by spray granulation-fluidized bed drying method to obtain lutein ester and zeaxanthin compound microcapsule with a particle size of 40-100 mesh.

[0023] Further, the heating temperature in step (1) is 65-85℃; the zeaxanthin content in step (1) is ≥50%, and the lutein ester content in step (2) is ≥50%. It should be noted that the content referred to in the present application refers to purity. As mentioned above, the purity of zeaxanthin and lutein ester on the market cannot reach 100%, and it is preferred to use those with a purity of not less than 50%.

[0024] Further, in step (3), the high-speed shearing speed is 7500-8500r / min, and the emulsification time is 50-60min; the homogenization pressure is 45-90MPa; the grinding adopts a ceramic sand mill with a rotation speed of 2500-3200r / min, the ground emulsion particle size is 100-500nm, and the PDI value is <0.3.

[0025] Further, in step (4), the spray granulation-fluidized bed drying method has the following conditions: the spray inlet air temperature is 160-180℃, and the fluidized bed air blowing temperature is 75-95℃.

[0026] Specifically, in some embodiments of the present application, the fluidized bed is filled with corn starch, and the corn starch feeding amount is 3-5 times the mass of the liquid, and the corn starch is circulated in the system during the spray granulation process to exchange heat and mass with the atomized droplets and to coat the lutein ester and zeaxanthin compound microcapsule.

[0027] In the preparation method, the filler is combined with the wall material to increase the embedding effect of the wall material on the lutein ester and the zeaxanthin. The combination of the compound emulsifier and the nanometer grinding technology can better solve the problem of difficult simultaneous emulsification of the lutein ester and the zeaxanthin due to different polarities. Further, the particle size of the grinding liquid is controlled to be 100-500 nm, thereby being beneficial to improving the bioavailability.

[0028] It should be noted that in the preparation method, the zeaxanthin can be nanometer ground, but the lutein ester cannot be directly nanometer ground, that is, nanometer grinding can be performed in step (1), and nanometer grinding cannot be performed in step (2), and nanometer grinding needs to be performed again after emulsification and homogenization, that is, grinding is performed again in step (3).

[0029] The lutein ester and zeaxanthin compound microcapsule prepared by the method has the effects of effectively protecting the eyes, preventing eye diseases, relieving eye fatigue, and improving the eyesight, and has good stability. After being placed at 40 DEG C and RH 75% for 3 months, the content retention rate is more than 95%.

[0030] In a third aspect, the application provides a functional food with an eye-protecting effect, which comprises the lutein ester and zeaxanthin compound microcapsule.

[0031] The functional food is a food with a specific nutritional and health-care function. The functional food comprises the lutein ester and zeaxanthin compound microcapsule, and thus has the effects of preventing visual fatigue and preventing cataract. The functional food can be added with other allowed auxiliary materials to form various dosage forms, such as capsules and tablets.

[0032] The application provides a lutein ester and zeaxanthin compound microcapsule, a preparation method and application thereof. The lutein ester and zeaxanthin compound microcapsule has the same proportion of lutein and zeaxanthin in the eyes of people, good stability, high bioavailability, and can be directly used or further processed into products in different dosage forms such as capsules and tablets. DETAILED DESCRIPTION

[0033] The technical solutions in the application will be described below in a clear and complete manner. Obviously, the described embodiments are only part of the embodiments of the application, rather than all the embodiments. Based on the embodiments in the application, all other embodiments obtained by those skilled in the art without creative work fall within the protection scope of the application.

[0034] Unless otherwise specified in the examples, the preparation process of the complex emulsifier is as follows:

[0035] Unless otherwise specified, the preparation process of the complex emulsifier in the following examples is as follows:

[0036] Glycerol monostearate, sorbitan monostearate and sucrose fatty acid ester were added to ethyl acetate, and the total mass of the three emulsifiers was 1:1 compared to the mass of ethyl acetate. The mixture was heated to dissolve at 50°C, and then concentrated to a residual amount of ethyl acetate ≤25 ppm after ultrasonic treatment for 20-25 min.

[0037] Example 1

[0038] In this example, lutein ester with a purity of 95% and zeaxanthin with a purity of 80% were selected as raw materials to provide a lutein ester and zeaxanthin complex microcapsule, and the preparation method was as follows:

[0039] (1) 460 g of gelatin, 379 g of white sugar, 15 g of zeaxanthin, and 25 g of complex emulsifier (glycerol monostearate 12.5 g, sorbitan monostearate 5 g, sucrose fatty acid ester 7.5 g) were added to 1000 g of purified water. The mixture was stirred at 75°C for 50 min until completely dissolved, and then nanomilled at 3000 rpm for one pass to obtain the water phase.

[0040] (2) 100 g of lutein ester was added to 10 g of medium-chain triglyceride and 11 g of vitamin E, and the mixture was stirred at 80°C for 30 min until completely dissolved to obtain the oil phase.

[0041] (3) The oil phase was slowly added to the water phase under high-speed shearing, and the shearing speed was 8000 r / min, and the emulsification time was 55 min. Then, the mixture was passed through two high-pressure homogenizers at a pressure of 75 MPa, and then nanomilled at 3000 rpm for three passes to obtain a milled emulsion with a particle size of 100-150 nm and a PDI value of 0.104.

[0042] (4) The emulsion was subjected to one-step granulation by spray granulation-fluidized bed drying method, and the spray drying conditions were as follows: inlet air temperature 165°C, fluidized bed air blowing temperature 95°C, to obtain microcapsules with a particle size of 40-100 mesh, a lutein ester content of 11.20%, and a zeaxanthin content of 1.35%.

[0043] Example 2

[0044] In this example, lutein ester with a purity of 95% and zeaxanthin with a purity of 80% were selected as raw materials to provide a lutein ester and zeaxanthin complex microcapsule, and the preparation method was as follows:

[0045] (1) 460 g gum arabic, 375.8 g maltose, 14 g zeaxanthin and 25 g compound emulsifier (glycerol monostearate 11.5 g, sorbitan monostearate 5 g, sucrose fatty acid ester 8.5 g) were added to 800 g purified water, stirred at 75 °C for 50 min until completely dissolved, and nano-milled once at 2800 rpm to prepare the water phase.

[0046] (2) 100 g lutein ester was added to 13 g medium-chain triglyceride and 12.2 g rosemary extract, stirred at 82 °C for 35 min until completely dissolved to prepare the oil phase.

[0047] (3) The oil phase was slowly added to the water phase under high-speed shearing, the shearing speed was 7500 r / min, the emulsification time was 55 min; then passed through two high-pressure homogenizers, the homogenization pressure was 90 MPa, then nano-milled twice at 3200 rpm, the particle size was 150-200 nm, and the PDI value was 0.217.

[0048] (4) The emulsion was one-step granulated by the spray granulation-fluidized bed drying method, the spray drying conditions were: inlet air temperature 160 °C, fluidized bed air blowing temperature 80 °C, to obtain the microcapsules with a particle size of 40-100 mesh, wherein the lutein ester content was 10.75%, and the zeaxanthin content was 1.19%.

[0049] Example 3

[0050] In this example, lutein ester with a purity of 90% and zeaxanthin with a purity of 70% were selected as raw materials, and a lutein ester and zeaxanthin compound microcapsule was provided, and the preparation method was as follows:

[0051] (1) 370 g modified starch, 438.5 g maltodextrin, 16.5 g zeaxanthin and 25 g compound emulsifier (glycerol monostearate 12.5 g, sorbitan monostearate 3.75 g, sucrose fatty acid ester 8.75 g) were added to 750 g purified water, stirred at 75 °C for 50 min until completely dissolved, and nano-milled once at 2800 rpm to prepare the water phase.

[0052] (2) 100 g lutein ester was added to 35 g medium-chain triglyceride and 15 g vitamin E, stirred at 85 °C for 35 min until completely dissolved to prepare the oil phase.

[0053] (3) The oil phase was slowly added to the water phase under high-speed shearing, the shearing speed was 7500 r / min, the emulsification time was 55 min; then passed through two high-pressure homogenizers, the homogenization pressure was 80 MPa, then nano-milled once at 2600 rpm, the particle size was 200-500 nm, and the PDI value was 0.289.

[0054] (4) The emulsion is granulated by spray granulation-fluidized bed drying method in one step, the spray drying conditions are: inlet air temperature 164℃, fluidized bed air blowing temperature 85℃, to obtain microcapsules with particle size of 40-100 mesh, wherein the lutein ester content is 10.46%, and the zeaxanthin content is 1.39%.

[0055] Example 4

[0056] In this example, lutein ester with a purity of 90% and zeaxanthin with a purity of 70% are selected as raw materials, and a lutein ester and zeaxanthin compound microcapsule is provided, and the preparation method is as follows:

[0057] (1) 365g modified starch, 443.5g malt dextrin, 16.5g zeaxanthin and 25g compound emulsifier (glycerol monostearate 12.5g, sorbitan monostearate 3.75g, sucrose fatty acid ester 8.75g, the three emulsifiers are directly added, without adding ethyl acetate and ultrasonic step) are added to 750g purified water, stirred at 75℃ for 50min until completely dissolved, nanomilled once at 2800rpm, to prepare the water phase.

[0058] (2) 100g lutein ester is added to 35g medium-chain triglyceride and 15g vitamin E, stirred at 85℃ for 35min until completely dissolved, to prepare the oil phase.

[0059] (3) The oil phase is slowly added to the high-speed sheared water phase, the shearing speed is 7500r / min, the emulsification time is 55min; then passed through two high-pressure homogenizers, the homogenization pressure is 80MPa, then nanomilled once at 2600rpm, the particle size is 500-1000nm, and the PDI value is 0.691.

[0060] (4) The emulsion is granulated by spray granulation-fluidized bed drying method in one step, the spray drying conditions are: inlet air temperature 170℃, fluidized bed air blowing temperature 95℃, to obtain microcapsules with particle size of 40-100 mesh, wherein the lutein ester content is 10.53%, and the zeaxanthin content is 1.42%.

[0061] On the basis of the above four examples, the ratio of lutein ester and zeaxanthin can be adjusted according to actual needs to obtain different compound microcapsules with a mass ratio of lutein ester to zeaxanthin in the range of 10:1-5:1.

[0062] The obtained compound microcapsules can be directly packaged, or can be further processed into different dosage forms such as capsules, tablets, etc. for use by different groups of people.

[0063] Comparative Example 1

[0064] Comparative Example 1

[0065] Comparative Example 2

[0066] Comparative Example 2

[0067] Comparative Example 3

[0068] Comparative Example 3

[0069] Comparative Example 4

[0070] Comparative Example 4

[0071] Comparative Example 5

[0072] Comparative Example 5

[0073] Comparative Example 6

[0074] Comparative Example 6

[0075] Comparative Example 7

[0076] Comparative Example 7

[0077] Storage stability experiment of Experimental Example 1

[0078] The microcapsule samples prepared in each example and the comparative example were taken respectively, and their appearance was observed, their particle size, PDI value (a dimensionless value reflecting the width of particle size distribution, ranging from 0 to 1, the smaller the value, the more uniform the particle size, and the more concentrated the particle size distribution), initial content of lutein ester, and content retention rate (lutein ester) after being placed at 40℃, RH 75% for 1 month, 2 months and 3 months, respectively, were measured. Among them, the content detection refers to the international JECFA standard "LUTEIN ESTERS FROM TAGETESERECTA". The results are shown in Table 1.

[0079] Table 1

[0080]

[0081]

[0082] Experimental Example 2: Bioavailability test

[0083] The microcapsule samples prepared in each example and the comparative example were taken respectively, and their appearance was observed, their particle size, PDI value (a dimensionless value reflecting the width of particle size distribution, ranging from 0 to 1, the smaller the value, the more uniform the particle size, and the more concentrated the particle size distribution), initial content of lutein ester, and content retention rate (lutein ester) after being placed at 40℃, RH 75% for 1 month, 2 months and 3 months, respectively, were measured. Among them, the content detection refers to the international JECFA standard "LUTEIN ESTERS FROM TAGETESERECTA". The results are shown in Table 1.

[0084] Table 2

[0085]

[0086]

[0087] From the above results, it can be seen that by using the complex emulsifier with a specific composition and the preparation process, the uniform emulsification effect of lutein ester and zeaxanthin is enhanced, thereby providing a complex microcapsule with the same proportion of lutein and zeaxanthin in the eyes of people, which has good stability and high bioavailability.

[0088] It should be noted that the endpoints of the ranges and any values disclosed herein are not limited to the precise values stated. The ranges and values should be interpreted as being approximate. For numeric values, the endpoints of each range, the endpoints of each range and individual point values, and individual point values can be combined with each other to form one or more new numeric ranges, which should be considered as being specifically disclosed herein.

[0089] In the description of the specification, the description of the terms "one embodiment", "some embodiments", "specific embodiments", or "some specific embodiments" etc. means that the specific features, structures, materials or characteristics described in connection with the embodiment or example are contained in at least one embodiment or example of the embodiments of the present application. In the specification, the illustrative description of the above terms does not necessarily refer to the same embodiment or example. Moreover, the specific features, structures, materials or characteristics described can be combined in any appropriate manner in any one or more embodiments or examples. In addition, the person skilled in the art can combine and combine the different embodiments or examples described in the specification and the features of the different embodiments or examples without contradiction.

[0090] Finally, it should be noted that: the above embodiments are only used to illustrate the technical solutions of the present application, and not to limit them; although the present application has been described in detail with reference to the foregoing embodiments, those skilled in the art should understand that: it can still modify the technical solutions recorded in the foregoing embodiments, or make equivalent replacement for part of the technical features; and these modifications or replacements do not make the essence of the corresponding technical solution deviate from the spirit and scope of the technical solutions of the embodiments of the present application.

Claims

1. A compound microcapsule of lutein ester and zeaxanthin, characterized in that, The lutein ester and zeaxanthin include lutein ester and zeaxanthin with a mass ratio of (5-10):1, a wall material, a filler, a compound emulsifier, an oil-soluble antioxidant, vegetable oil and pure water, the compound emulsifier is glycerol monostearate, sorbitan monostearate and sucrose fatty acid ester with a mass ratio of (4.2-5):(1.5-2):(2.6-3.5); The preparation method of the compound emulsifier is: glycerol monostearate, sorbitan monostearate and sucrose fatty acid ester are added into ethyl acetate, the mass ratio of the total mass of the three emulsifiers to the mass of ethyl acetate is 1:1, heated and dissolved at 50 DEG C, and after ultrasonic treatment for 20-25 min, concentrated to the residual amount of ethyl acetate ≤25 ppm; The lutein ester and zeaxanthin compound microcapsule includes the following components by weight: The lutein ester and zeaxanthin compound microcapsule includes the following components by weight: The preparation method of the lutein ester and zeaxanthin compound microcapsule includes the following steps: (1) the wall material, the filler, the compound emulsifier, the zeaxanthin are added into the pure water, heated and stirred to dissolve, and the water phase is prepared by nanometer grinding at 2800 rpm-3000 rpm; (2) the lutein ester is melted in the mixture of the vegetable oil and the oil-soluble antioxidant to prepare the oil phase; (3) the oil phase is added into the water phase with high-speed shearing to emulsify, then homogenized, and the homogenized emulsion is ground to obtain the ground emulsion; the grinding speed is 2500-3200 r / min, the particle size of the ground emulsion is 100-500 nm, and the PDI value is <0.3; The wall material is one or more of sodium alginate, gum arabic, modified starch and gelatin; The filler is one or more of sucrose, maltose, oligomeric isomaltose and malt dextrin; The oil-soluble antioxidant is any one of vitamin E and rosemary extract; The vegetable oil is one or more of grape seed oil, soybean oil, safflower seed oil and medium-chain triglyceride.

2. The lutein ester and zeaxanthin complex microcapsule according to claim 1, characterized by, The lutein ester content in the lutein ester and zeaxanthin compound microcapsule is ≥10%, and the zeaxanthin content is ≥1%; the microcapsule particle size is between 40-100 mesh.

3. Process for the preparation of lutein ester and zeaxanthin complex microcapsules according to any one of claims 1-2, characterized in that, The preparation method of the lutein ester and zeaxanthin compound microcapsule includes the following steps: (1) the wall material, the filler, the compound emulsifier, the zeaxanthin are added into the pure water, heated and stirred to dissolve, and the water phase is prepared by nanometer grinding at 2800 rpm-3000 rpm; (2) the lutein ester is melted in the mixture of the vegetable oil and the oil-soluble antioxidant to prepare the oil phase; (3) the oil phase is added into the water phase with high-speed shearing to emulsify, then homogenized, and the homogenized emulsion is ground to obtain the ground emulsion; the grinding speed is 2500-3200 r / min, the particle size of the ground emulsion is 100-500 nm, and the PDI value is <0.3; (4) the ground emulsion is granulated by the spray granulation-fluidized bed drying method to obtain the lutein ester and zeaxanthin compound microcapsule with a particle size of 40-100 mesh.

4. The method of claim 3, wherein the preparation of the lutein ester and zeaxanthin complex microcapsule is characterized by, The heating temperature in the step (1) is 65-85℃; the content of zeaxanthin in the step (1) is ≥50%, and the content of lutein ester in the step (2) is ≥50%.

5. The method of claim 3, wherein the preparation of the lutein ester and zeaxanthin complex microcapsule is characterized by, In the step (3), the high-speed shearing speed is 7500-8500r / min, the emulsification time is 50-60min, the homogenization pressure is 45-90MPa, and the grinding is carried out by using a ceramic sand mill.

6. The method of claim 3, wherein the preparation of the lutein ester and zeaxanthin complex microcapsule is characterized by, In the step (4), the spray granulation-fluidized bed drying method is carried out under the conditions that the spray inlet air temperature is 160-180℃, and the fluidized bed air blowing temperature is 75-95℃.

7. A functional food having an eye-protecting effect, characterized by comprising the extract of claim 1. The lutein ester and zeaxanthin compound microcapsule of any one of claims 1-2.

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