A carotenoid preparation composition and preparation method thereof

Abstract

The present invention provides a composition of a carotenoid preparation and a preparation method thereof. The carotenoid preparation in the composition is prepared by the following method: the carotenoid crystals are pre-treated and mixed with a gelled wall material, and then embedded once and twice to obtain the carotenoid preparation; the composition includes lutein and zeaxanthin; the mass ratio of the lutein to zeaxanthin is 1:(1.5-2.5). The present invention combines lutein and zeaxanthin in a specific ratio, and the resulting composition not only has a lower pigment solubility, but also has good antioxidant and blue light damage resistance effects.

Description

Technical Field

[0001] The present invention belongs to the technical field of particle preparation, and in particular relates to a composition of a carotenoid preparation and a preparation method thereof. Background Art

[0002] Carotenoids are a class of yellow, orange-red or red polyene substances, generally composed of 8 isoprenoid units, with a molecular formula of C 40 H 56 . Carotenoids are the most widely distributed pigments in nature. Vitamin A in the human body mainly comes from carotenoids. Carotenoids can help the human body prevent night blindness, maintain the stability of cell membranes, and resist adverse environments. Lutein, one of the components of carotenoids, is the main pigment that constitutes the macular area of the human retina, and plays a positive role in maintaining eye health and protecting vision. At the same time, carotenoids are a physiological antioxidant that can hinder the peroxidation of lipids, thereby protecting the steroid-producing cells of the follicles and uterus from oxidation. However, carotenoids are insoluble in water and have very low solubility in fats and oils. At the same time, they are unstable to light, oxygen, and heat, which limits their application. Conventional methods microencapsulate carotenoids to form encapsulated products to improve their bioavailability and also improve their coloring ability. For example, the colors of some desserts and beverages come from carotenoids.

[0003] CN114287625A discloses a carotenoid preparation and its application. The preparation comprises a mixture of pretreated carotenoid and pretreated gelling wall material, followed by emulsification and granulation to produce a powder or granular product. This method reduces pigment dissolution and ensures sustained release and stable efficacy during use. However, its biological activity has not been verified. In addition to reducing pigment dissolution, carotenoid preparations must also maintain biological activity during use.

[0004] CN107136503A discloses a method for preparing starch-embedded lutein microcapsules. This method involves heating a starch milk of a certain concentration to expand for 0.5 to 2 hours to form expanded starch. A solvent containing lutein is then added dropwise while the mixture is kept warm and stirred. The mixture reacts for 0.5 to 4 hours, then cooled. The mixture is recrystallized at 4 to 25°C for 4 to 12 hours, centrifuged, washed, and dried to obtain lutein microcapsules. After a three-week storage stability test, the lutein retention rate reached 72.1%, and the release rate in human intestinal fluid conditions reached 87.2%, achieving targeted intestinal sustained release and facilitating lutein absorption and utilization by the human body. However, the microcapsules produced by this method have a relatively large particle size, which limits their practical application.

[0005] Therefore, developing a carotenoid preparation composition that can effectively control pigment dissolution, ensure biological activity and have a high release rate is a research focus in this field. Summary of the Invention

[0006] In view of the shortcomings of the prior art, the present invention aims to provide a carotenoid preparation composition and a preparation method thereof, which can effectively control the dissolution of the pigment, ensure biological activity and have a high release rate.

[0007] In order to achieve the purpose of the invention, the present invention adopts the following technical solutions:

[0008] In a first aspect, the present invention provides a composition of a carotenoid preparation, wherein the carotenoid preparation in the composition is prepared by the following method, comprising: pre-treating carotenoid crystals, mixing them with a gelling wall material, and performing primary embedding and secondary embedding to obtain the carotenoid preparation;

[0009] The composition includes lutein and zeaxanthin;

[0010] The mass ratio of the lutein to the zeaxanthin is 1:(1.5-2.5).

[0011] The present invention effectively improves the stability of carotenoid crystals after pretreatment and maintains their biological activity. After a primary embedding, the pigment dissolution is effectively reduced and the release rate is increased. After a secondary embedding, the pigment dissolution is further reduced with almost no effect on the biological activity, thereby expanding the application of the product of the present invention in actual production and life.

[0012] Among them, 1:(1.5-2.5) can be, for example, 1:1.6, 1:1.8, 1:2, 1:2.2, 1:2.4, etc.

[0013] In the present invention, the zeaxanthin used contains two isomers, (3R, 3'R) zeaxanthin and (3R, 3'S) zeaxanthin, and the weight ratio between the two isomers is (5-15): (95-85).

[0014] Preferably, the raw materials of the composition further include perilla seed oil.

[0015] Preferably, the mass ratio of lutein, zeaxanthin and perilla seed oil in the composition is 1:(1.5-2.5):(0.2-2), for example, it can be 1:1.6:0.2, 1:1.8:0.2, 1:2:0.2, 1:2.2:0.2, 1:2.4:0.2, 1:1.6:0.8, 1:1.8:0.8, 1:2:0.8, 1:2.2:0.8, 1:2.4:0.8, 1:1.6:1.5, 1:1.8:1.5, 1:2:1.5, 1:2.2:1.5, 1:2.4:1.5, and the like.

[0016] In the present invention, perilla seed oil is embedded once in the same manner as carotenoids. During secondary embedding, the primary embedding product of perilla seed oil and the primary embedding product of carotenoids can be mixed, and then the mixture is embedded twice to obtain a carotenoid preparation composition; or the primary embedding product of perilla seed oil is embedded twice alone to obtain a secondary embedding product of perilla seed oil, and then the secondary embedding product of perilla seed oil and the secondary embedding product of carotenoids are mixed to obtain a carotenoid preparation composition.

[0017] Preferably, the median particle size D of the composition 50 ≤150μm, for example, it can be 145μm, 140μm, 135μm, 130μm, 125μm, 120μm, 115μm, 110μm, 105μm, 100μm, etc.

[0018] Preferably, the pretreatment method comprises the following steps: mixing carotenoid crystals with an ethanol aqueous solution, stirring and dispersing, adding an antioxidant and then removing the solvent to obtain pretreated carotenoid crystals.

[0019] Preferably, the mass ratio of the carotenoid crystals to the ethanol aqueous solution is 1:(3-5), for example, 1:3.5, 1:4, 1:4.5, etc.

[0020] Preferably, the mass percentage of ethanol in the ethanol aqueous solution is 50-70%, for example, 55%, 60%, 65%, etc.

[0021] Preferably, the antioxidant comprises any one or a combination of at least two of ascorbic acid, ascorbyl palmitate, sucrose fatty acid esters, tocopherol, fatty acid ascorbic acid esters, butylated hydroxytoluene, butylated hydroxyanisole, propyl gallic acid or tert-butylhydroxyquinoline.

[0022] Preferably, the ethanol residual content in the pretreated carotenoid crystals is less than 10 ppm, for example, it may be 8 ppm, 6 ppm, 4 ppm, 2 ppm, etc.

[0023] Preferably, the water content of the pretreated carotenoid crystals is 10-30%, for example, 15%, 20%, 25%, etc.

[0024] Preferably, the total pigment content in the pretreated carotenoid crystals is ≥80%, for example, it can be 82%, 84%, 86%, 88%, 90%, 92%, 94%, etc.

[0025] Preferably, the method for preparing the gelled wall material comprises the following steps: dissolving the wall material and carbohydrate to obtain an aqueous solution, and dispersing, stirring, and gelling the aqueous solution to obtain the gelled wall material.

[0026] Preferably, the mass ratio of the wall material to the carbohydrate is (1-5):1, for example, 2:1, 3:1, 4:1, etc.

[0027] Preferably, the wall material comprises any one or a combination of at least two of sodium starch octenylsuccinate, gum arabic or cellulose derivatives.

[0028] Preferably, the wall material is gum arabic.

[0029] Preferably, the carbohydrate comprises any one of sucrose, glucose, glucose syrup, xylose, malto-oligosaccharides, fructo-oligosaccharides or solid corn syrup, or a combination of at least two thereof.

[0030] Preferably, the carbohydrate is glucose.

[0031] Preferably, the primary embedding includes the steps of mixing, emulsification and drying.

[0032] Preferably, the emulsifier used in the emulsification treatment includes any one of sucrose fatty acid ester, Tween or Span, or a combination of at least two of them.

[0033] Preferably, the fat-soluble material used for the secondary embedding includes any one of hydrogenated vegetable oil, glycerol fatty acid ester, beeswax, carnauba wax or palm oil, or a combination of at least two thereof.

[0034] Preferably, the hydrogenated vegetable oil includes any one of hydrogenated palm oil, hydrogenated soybean oil, hydrogenated sunflower oil, hydrogenated peanut oil, hydrogenated cottonseed oil or hydrogenated corn oil, or a combination of at least two thereof.

[0035] Preferably, the glycerol fatty acid ester includes any one of mono- and diglycerol fatty acid esters, hexadecanoic acid glyceryl, hexadecenoic acid glyceryl, octadecanoic acid glyceryl, octadecenoic acid glyceryl, octadecadienoic acid glyceryl or octadecatrienoic acid glyceryl, or a combination of at least two thereof.

[0036] Preferably, the fat-soluble material is hydrogenated palm oil.

[0037] Preferably, the auto-melting point of the fat-soluble material is 45-90°C, for example, 50°C, 55°C, 60°C, 65°C, 70°C, 75°C, 80°C, 85°C, etc.

[0038] Preferably, the mass percentage of carotenoid crystals in the carotenoid preparation is 5-20%, for example, 7%, 10%, 12%, 14%, 16%, 18%, etc.

[0039] Preferably, the mass percentage of the wall material embedded once in the carotenoid preparation is 25-35%, for example, 26%, 28%, 30%, 32%, 34%, etc.

[0040] Preferably, the mass percentage of the secondary embedded fat-soluble material in the carotenoid preparation is 30-55%, for example, 35%, 40%, 45%, 50%, etc.

[0041] The numerical range described in the present invention includes not only the point values listed above, but also any point values between the above numerical ranges that are not listed. Due to space limitations and for the sake of simplicity, the present invention no longer exhaustively lists the specific point values included in the range.

[0042] In a second aspect, the present invention provides a method for preparing the carotenoid preparation composition according to the first aspect, the preparation method comprising the following steps:

[0043] (1) mixing carotenoid crystals with an ethanol aqueous solution, stirring and dispersing, adding an antioxidant and removing the solvent to obtain pretreated carotenoid crystals;

[0044] (2) dissolving the wall material and the carbohydrate to obtain an aqueous solution, and dispersing, stirring, and gelling the aqueous solution to obtain a gelled wall material;

[0045] (3) mixing the pretreated carotenoid crystals with a gelling wall material, emulsifying and drying to obtain a primary encapsulation product;

[0046] (4) melting the fat-soluble material, mixing it with the primary embedding product, and atomizing it to prepare the carotenoid preparation composition;

[0047] The order of steps (1) and (2) is not limited;

[0048] Preferably, in step (1), the stirring temperature is 40-50°C, for example, 42°C, 44°C, 46°C, 48°C, etc., and the stirring time is at least 20 minutes, for example, 25 minutes, 30 minutes, 35 minutes, 40 minutes, 45 minutes, 50 minutes, etc.

[0049] Preferably, the temperature for removing the solvent is 70-80°C, for example, 72°C, 74°C, 76°C, 78°C, etc.

[0050] Preferably, the mass percentage of soluble solids in the aqueous solution is 50-70%, for example, 55%, 60%, 65%, etc.

[0051] Preferably, in step (2), the dispersion temperature is 50-70°C, for example, 55°C, 60°C, 65°C, etc.

[0052] Preferably, in step (2), the stirring temperature is 80-90°C, for example, 82°C, 84°C, 86°C, 88°C, etc., and the stirring time is 35-50min, for example, 36min, 38min, 40min, 42min, 44min, 46min, 48min, etc.

[0053] Preferably, the gelation temperature is 60-65°C, for example, 61°C, 62°C, 63°C, 64°C, etc., and the gelation time is 110-130 min, for example, 115 min, 120 min, 125 min, etc.

[0054] Preferably, the atomization pressure is 0.2-0.4 MPa, for example, 0.25 MPa, 0.3 MPa, 0.35 MPa, etc., and the temperature of the material during atomization is 13-17°C, for example, 14°C, 15°C, 16°C, etc.

[0055] Preferably, the preparation method comprises the following steps:

[0056] (1) mixing carotenoid crystals with an ethanol aqueous solution, stirring at 40-50° C. for at least 20 minutes, adding an antioxidant after dispersion, and removing the solvent at 70-80° C. to obtain pretreated carotenoid crystals;

[0057] (2) dissolving the wall material and carbohydrate to obtain an aqueous solution having a soluble solid content of 50-70% by weight, dispersing the aqueous solution at 50-70° C., stirring at 80-90° C. for 35-50 minutes, and gelling at 60-65° C. for 110-130 minutes to obtain a gelled wall material;

[0058] (3) mixing the pretreated carotenoid crystals with a gelling wall material, emulsifying and drying to obtain a primary encapsulation product;

[0059] (4) melting the fat-soluble material and mixing it with the primary embedding product, and atomizing the mixture at a pressure of 0.2-0.4 MPa, wherein the temperature of the material during atomization is 13-17° C., to prepare the carotenoid preparation composition;

[0060] There is no limitation on the order of steps (1) and (2).

[0061] In a third aspect, the present invention provides a use of the carotenoid preparation composition as described in the first aspect in food, beverages, health products or medicines.

[0062] Compared with the prior art, the present invention has the following beneficial effects:

[0063] 1. The present invention combines lutein and zeaxanthin in a specific ratio to obtain a composition with good antioxidant and blue light damage protection effects. Furthermore, lutein, zeaxanthin and perilla seed oil are combined in a specific ratio, and the three work synergistically to jointly promote the antioxidant and blue light damage protection effects of the composition. Animal experiments show that after blue light damage, the decrease in malondialdehyde (MDA) of the composition is more than 13.5 times that of lutein or zeaxanthin alone.

[0064] 2. The present invention pre-treats carotenoids and then performs a primary embedding, which effectively improves their stability and release rate while maintaining their biological activity and effectively reducing pigment dissolution. A secondary embedding is performed, and pigment dissolution is further reduced. The pigment solubility of the carotenoid preparation of the present invention is less than 1%, which has almost no effect on biological activity, thereby expanding the application of the composition product of the present invention in actual production and life. DETAILED DESCRIPTION

[0065] 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.

[0066] 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.

[0067] "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.

[0068] 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.

[0069] 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.

[0070] The sources of reagents or instruments in the following examples are as follows:

[0071] Lutein crystals: total pigment content is 86%, and the liquid phase content of trans-lutein is 93%;

[0072] Zeaxanthin crystals: provided by Dalian Yinuo Biological Co., Ltd., with a zeaxanthin content of 72.7%;

[0073] Perilla seed oil: provided by Dalian Yinuo Biological Co., Ltd.

[0074] Preparation Example 1

[0075] This preparation example provides a mixture, wherein the raw materials of the mixture include: 100g of lutein crystals, 220g of zeaxanthin crystals, and 80g of perilla seed oil; the above raw materials are mixed and crushed according to the formula amount to obtain the mixture.

[0076] Preparation Example 2

[0077] This preparation example provides a mixture, wherein the raw materials of the mixture include: 100g lutein crystals, 166g zeaxanthin crystals, and 64g perilla seed oil; the above raw materials are mixed and crushed according to the formula amount to obtain the mixture.

[0078] Preparation Example 3

[0079] This preparation example provides a mixture, wherein the raw materials of the mixture include: 100g of lutein crystals, 275g of zeaxanthin crystals, and 16g of perilla seed oil; the above raw materials are mixed and crushed according to the formula amount to obtain the mixture.

[0080] Preparation Example 4

[0081] This preparation example provides a mixture, which differs from Preparation Example 1 only in that perilla seed oil is replaced with an equal amount of hydrogenated palm oil; other raw materials, amounts and preparation methods are the same as those in Preparation Example 1.

[0082] Preparation Example 5

[0083] This preparation example provides a mixture, wherein the raw materials of the mixture include: 100g of lutein crystals, 110g of zeaxanthin crystals, and 80g of perilla seed oil; the above raw materials are mixed and crushed according to the formula amount to obtain the mixture.

[0084] Preparation Example 6

[0085] This preparation example provides a mixture, wherein the raw materials of the mixture include: 100g of lutein crystals, 55g of zeaxanthin crystals, and 40g of perilla seed oil; the above raw materials are mixed and crushed according to the formula amount to obtain the mixture.

[0086] Preparation Example 7

[0087] This preparation example provides a mixture, wherein the raw materials of the mixture include: 100g of lutein crystals, 220g of zeaxanthin crystals, and 200g of perilla seed oil; the above raw materials are mixed and crushed according to the formula amount to obtain the mixture.

[0088] Comparative Preparation Example 1

[0089] This comparative preparation example provides a mixture, wherein the raw materials of the mixture include: 100 g of lutein crystals and 80 g of perilla seed oil; the above raw materials are mixed and crushed according to the formula amount to obtain the mixture.

[0090] Comparative Preparation Example 2

[0091] This comparative preparation example provides a mixture, wherein the raw materials of the mixture include: 220 g of zeaxanthin crystals and 80 g of perilla seed oil; the above raw materials are mixed and crushed according to the formula amount to obtain the mixture.

[0092] Test Example 1

[0093] Oxidative damage test-cell experiment

[0094] ARPE-19 ocular cells in logarithmic growth phase were cultured at 1.5×10 5 Each well was evenly inoculated into a 6-well plate and cultured for 24 h as a blank control group;

[0095] Hydrogen peroxide group: ARPE-19 ocular cells in the logarithmic growth phase were cultured at a concentration of 1.5×10 5 Cells were evenly seeded into 6-well plates, cultured for 24 h, and treated with hydrogen peroxide (300 μM) for 4 h to induce oxidative damage;

[0096] Treatment group: ARPE-19 ocular cells in the logarithmic growth phase were cultured at a rate of 1.5×10 5Cells were evenly seeded into 6-well plates, cultured for 24 h, and 20 μM of the mixture of the preparation example, the comparative preparation example, lutein crystals or zeaxanthin crystals were added respectively for 24 h. Oxidative damage was induced by treating with hydrogen peroxide (300 μM) for 4 h.

[0097] The above three groups were detected by flow cytometry at 488 nm excitation wavelength and 525 nm emission wavelength to detect the fluorescence peaks of each group, thereby reflecting the level of reactive oxygen species (ROS).

[0098] Results Analysis: Flow cytometry data were processed using FlowJo software to determine fluorescence intensity, which represents ROS levels and thus reflects antioxidant levels. The test results are shown in Table 1.

[0099] Test Example 2

[0100] Blue light damage resistance test-cell experiment

[0101] ARPE-19 ocular cells in logarithmic growth phase were cultured at 1.5×10 6 The cells / dish were evenly inoculated into 6 cm culture dishes and cultured for 24 h as the blank control group;

[0102] Blue light group: ARPE-19 ocular cells in the logarithmic growth phase were treated with 1.5×10 6 The cells were evenly inoculated into 6 cm culture dishes, cultured for 24 h, and irradiated with 4000-5333 Lux blue light for 2 h to induce blue light damage.

[0103] Treatment group: ARPE-19 ocular cells in the logarithmic growth phase were cultured at a rate of 1.5×10 6 Each cell was evenly inoculated into a 6 cm culture dish and cultured for 24 h. 20 μM of the mixture of the preparation example, the comparative preparation example, lutein crystals or zeaxanthin crystals were added respectively and treated for 24 h. The cells were then irradiated with 4000-5333 Lux blue light for 2 h to induce blue light damage.

[0104] The above three groups detected the peak diagram of the cell cycle by flow cytometry to reflect the level of each cycle.

[0105] Results Analysis: Flow cytometry data was processed using FlowJo software to determine the proportions of each cell cycle phase. The G2 / M phase ratio was used as an indicator to reflect the level of resistance to blue light damage. The test results are shown in Table 1.

[0106] Table 1

[0107]

[0108]

[0109] It can be seen from Preparation Examples 1-3 and Preparation Examples 5-7 that when the content ratio of lutein, zeaxanthin and perilla seed oil in the mixture is 1:(1.5-2.5):(0.2-2), the antioxidant and blue light damage resistance effects are better, and from Preparation Example 4, it can be seen that when perilla seed oil is not added and the combination ratio of lutein and zeaxanthin is 1:2, its antioxidant effect and blue light damage resistance effect are also good; it can be seen from Preparation Example 1 and Comparative Preparation Examples 1-2 that when the raw material lacks lutein crystals or zeaxanthin, its antioxidant and blue light damage resistance effects are poor; it can be seen from Preparation Example 1 and lutein crystals and zeaxanthin crystals that when the raw material only contains lutein or zeaxanthin, it also has a certain antioxidant effect, but the effect is not good.

[0110] Example 1

[0111] This embodiment provides a composition of a carotenoid preparation, wherein the raw materials of the composition include: 100g of lutein crystals, 220g of zeaxanthin crystals, and 80g of perilla seed oil;

[0112] Preparation method:

[0113] (1) Lutein crystals and zeaxanthin crystals were mixed with 4 times the amount of 60% ethanol aqueous solution, stirred at 45°C for 30 minutes, and then dispersed by high-speed shearing at 10,000 rpm. 20 g of ascorbic acid, 1 g of ascorbyl palmitate, and 1 g of sucrose fatty acid ester were added. The solvent was removed at 75°C until the ethanol residue was 6 ppm and the water content of the crystals was 15%. Perilla seed oil was added and mixed uniformly to obtain a pretreated mixture.

[0114] (2) 432 g of gum arabic and 144 g of glucose were prepared into a 60% solid content aqueous solution, stirred and dispersed at 60°C, then heated to 85°C and stirred at a constant speed for 40 minutes. Cooled to 60°C and stirred for 120 minutes to obtain a gelled wall material;

[0115] (3) mixing and stirring the gelled wall material and the pretreated mixture obtained in step (1), emulsifying the mixture with 2 g of sucrose fatty acid ester, and spray drying the mixture to obtain a primary encapsulation product;

[0116] (4) 1000 g of hydrogenated palm oil was melted at 90° C. and mixed with the primary encapsulated product, stirred and dispersed evenly, and pumped into an atomizer at an atomization pressure of 0.3 MPa and a material temperature of 15° C. to obtain the composition of the carotenoid preparation.

[0117] Example 2

[0118] This embodiment provides a composition of a carotenoid preparation, wherein the raw materials of the composition include: 100g of lutein crystals, 166g of zeaxanthin crystals, and 64g of perilla seed oil;

[0119] Preparation method:

[0120] (1) Lutein crystals and zeaxanthin crystals were mixed with 3 times the amount of 70% ethanol aqueous solution, stirred at 40°C for 30 minutes, and then dispersed by high-speed shearing at 10,000 rpm. 20 g of ascorbic acid, 1 g of ascorbyl palmitate, and 1 g of sucrose fatty acid ester were added. The solvent was removed at 80°C until the ethanol residue was 8 ppm and the water content of the crystals was 17%. Perilla seed oil was added and mixed uniformly to obtain a pretreated mixture.

[0121] (2) 484.5 g of gum arabic and 161.5 g of glucose were prepared into a 50% solid content aqueous solution, stirred and dispersed at 50°C, then heated to 80°C and stirred at a constant speed for 50 min. Cooled to 60°C and stirred for 130 min to obtain a gelled wall material;

[0122] (3) mixing and stirring the gelled wall material and the pretreated mixture obtained in step (1), emulsifying the mixture with 3 g of sucrose fatty acid ester, and spray drying the mixture to obtain a primary encapsulation product;

[0123] (4) 1000 g of hydrogenated palm oil was melted at 90° C. and mixed with the primary encapsulated product, stirred and dispersed evenly, and pumped into an atomizer at an atomization pressure of 0.2 MPa and a material temperature of 17° C. to obtain the carotenoid preparation composition.

[0124] Example 3

[0125] This embodiment provides a composition of a carotenoid preparation, wherein the raw materials of the composition include: 100g of lutein crystals, 275g of zeaxanthin crystals, and 16g of perilla seed oil;

[0126] Preparation method:

[0127] (1) Lutein crystals and zeaxanthin crystals were mixed with 5 times the amount of 50% ethanol aqueous solution, stirred at 50°C for 20 minutes, and then dispersed by high-speed shearing at 10,000 rpm. 20 g of ascorbic acid, 1 g of ascorbyl palmitate, and 1 g of sucrose fatty acid ester were added. The solvent was removed at 70°C until the ethanol residue was 5 ppm and the water content of the crystals was 13%. Perilla seed oil was added and mixed uniformly to obtain a pretreated mixture.

[0128] (2) 438 g of gum arabic and 146 g of glucose were prepared into a 70% solid content aqueous solution, stirred and dispersed at 70°C, then heated to 90°C and stirred at a constant speed for 35 minutes. Cooled to 65°C and stirred for 110 minutes to obtain a gelled wall material;

[0129] (3) mixing and stirring the gelled wall material and the pretreated mixture obtained in step (1), emulsifying the mixture with 3 g of sucrose fatty acid ester, and spray drying the mixture to obtain a primary encapsulation product;

[0130] (4) 1000 g of hydrogenated palm oil was melted at 90° C. and mixed with the primary encapsulated product, stirred and dispersed evenly, and pumped into an atomizer at an atomization pressure of 0.4 MPa and a material temperature of 13° C. to obtain the carotenoid preparation composition.

[0131] Example 4

[0132] This embodiment provides a composition of a carotenoid preparation, which differs from Example 1 only in that perilla seed oil is replaced with an equal amount of hydrogenated palm oil; other raw materials and amounts are the same as those in Example 1.

[0133] Example 5

[0134] This embodiment provides a composition of a carotenoid preparation, which differs from Example 1 only in that the gum arabic in step (2) is replaced with an equal amount of sodium starch octenylsuccinate, and the other raw materials, amounts and preparation methods are the same as those in Example 1.

[0135] Example 6-1

[0136] This embodiment provides a composition of a carotenoid preparation, which differs from Example 1 only in that the hydrogenated palm oil in step (4) is replaced by an equal amount of hydrogenated soybean oil; other raw materials, amounts and preparation methods are the same as those in Example 1.

[0137] Example 6-2

[0138] This embodiment provides a composition of a carotenoid preparation, which differs from Example 1 only in that the hydrogenated palm oil in step (4) is replaced by an equal amount of carnauba wax; other raw materials, amounts and preparation methods are the same as those in Example 1.

[0139] Example 6-3

[0140] This embodiment provides a composition of a carotenoid preparation, which differs from Example 1 only in that the hydrogenated palm oil in step (4) is replaced with an equal amount of mono- and diglycerol fatty acid esters; other raw materials, amounts used, and preparation methods are the same as those in Example 1.

[0141] Example 6-4

[0142] This embodiment provides a composition of a carotenoid preparation, which differs from Example 1 only in that the hydrogenated palm oil in step (4) is replaced by an equal amount of beeswax; other raw materials, amounts and preparation methods are the same as those in Example 1.

[0143] Comparative Example 1

[0144] This comparative example provides a composition of a carotenoid preparation, which differs from Example 1 only in that zeaxanthin crystals and perilla seed oil are not added. While maintaining the total content of lutein, zeaxanthin, and perilla seed oil in the composition unchanged, the insufficient amount is supplemented by lutein crystals; other raw materials, amounts, and preparation methods are the same as in Example 1.

[0145] Comparative Example 2

[0146] This comparative example provides a carotenoid preparation composition, which differs from Example 1 only in that lutein crystals and perilla seed oil are not added. While maintaining the total content of lutein, zeaxanthin, and perilla seed oil in the composition unchanged, the insufficient amount is supplemented by zeaxanthin crystals; other raw materials, amounts, and preparation methods are the same as in Example 1.

[0147] Test Example 3

[0148] Pigment solubility determination

[0149] Get 1g of the composition of embodiment respectively and add 50mL water, 90 ℃, 100 revs, stirring and dissolving 30min, then filter and transfer in a volumetric flask, 30mL water washing once, combine filtrate, measure the OD value of maximum absorption wavelength after constant volume. Pigment dissolution is (OD value / product mass) × 100%. Test result is as shown in Table 2.

[0150] Table 2

[0151] Composition Dissolution (%) Particle size (D50, μm) Example 1 0.29 135 Example 2 0.30 133 Example 3 0.25 136 Example 4 0.4 127 Example 5 1.9 155 Example 6-1 0.6 157 Example 6-2 0.7 166 Example 6-3 1.3 150 Example 6-4 1.1 175

[0152] When testing the pigment solubility, the solubility of the primary embedded products in Examples 1-3 was checked, and the solubility of the primary embedded products was 2.8-3.4%. According to the table data, the two-step embedding process provided by the present invention can effectively reduce the pigment solubility of the product and further improve the user experience. It can be seen from Examples 1 and 4 that when the raw material lacks perilla seed oil, the pigment dissolution is slightly increased from 0.25-0.3 to 0.4; it can be seen from Examples 1 and 5 that when the wall material of the primary embedding does not use gum arabic, the solubility of the primary embedded product is 3.3%, but after the secondary embedding, its dissolution is lower than that of gum arabic. It can be seen from Examples 1 and 6 that when a fat-soluble material other than hydrogenated palm oil is used for the secondary embedding, its dissolution effect deteriorates and the product particle size increases to a certain extent.

[0153] Test Example 4

[0154] Anti-blue light damage test-animal experiment

[0155] Experimental animals:

[0156] 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 Laboratory Animal Ethics Committee (ethics number: AEE21112).

[0157] Drugs and reagents:

[0158] Malondialdehyde (MDA) kit, total superoxide dismutase (T-SOD) kit, and glutathione peroxidase (GSH-PX) kit were purchased from Nanjing Jiancheng Bioengineering Institute.

[0159] Experimental methods:

[0160] The establishment of the blue light damage model in mice and the administration of the composition were carried out. The mice were divided into groups according to the experimental group design, including:

[0161] Blank group: physiological saline was administered for 14 consecutive days, and then dark conditions were maintained for 12 h after the end of administration;

[0162] Blue light group: Normal saline was administered for 14 consecutive days, and then irradiated with blue light with an average illuminance of 4000-5333 Lux for 12 hours;

[0163] Experimental group: Each mouse was administered 20 mg / kg of the composition of each example and comparative example daily for 14 consecutive days. After the administration, the mice were irradiated with blue light of an average illumination of 4000-5333 Lux for 12 hours.

[0164] 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.

[0165] 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.

[0166] The calculation formula is:

[0167] T-SOD growth multiple = experimental group / blue light group - 1;

[0168] GSH-PX growth multiple = experimental group / blue light group - 1;

[0169] MDA reduction factor = blue light group / experimental group - 1. The test results are shown in Table 3.

[0170] Table 3

[0171] sample Proportion composition MDA decline multiple T-SOD growth multiple GSH-PX growth multiple Example 1 1:2:1 39.3 0.77 1.65 Example 4 1:2:0 38.54 0.71 1.60 Comparative Example 1 1:0:0 2.85 0.46 1.20 Comparative Example 2 0:1:0 2.82 0.60 1.14

[0172] Animal experiments on resisting blue light damage show that when the mass ratio of lutein, zeaxanthin and perilla seed oil in the raw materials is 1:2:1, the effect of resisting blue light damage is better, and the MDA reduction multiple is 13.8 times that of lutein or zeaxanthin alone. When the combined ratio of lutein and zeaxanthin is 1:2, the effect of resisting blue light damage is also good, and the MDA reduction multiple is 13.5 times that of lutein or zeaxanthin alone. It can be seen that the combination has an excellent effect in resisting blue light damage.

[0173] 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.

[0174] 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.

[0175] 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 carotenoid preparation composition, characterized in that: The raw materials of the composition include carotenoid crystals and perilla seed oil, wherein the carotenoid crystals are a combination of lutein and zeaxanthin. The composition is prepared by the following method, which includes: pre-treating the carotenoid crystals and perilla seed oil, mixing them with a gelling wall material, and performing primary and secondary embedding to obtain the carotenoid preparation composition; The fat-soluble material used in the secondary embedding is hydrogenated palm oil; The mass ratio of the lutein, zeaxanthin and perilla seed oil is 1:(1.5-2.5):(0.2-2).

2. The composition according to claim 1, characterized in that The particle size of the composition is ≤150 μm.

3. The composition according to claim 1, characterized in that The pretreatment method comprises the following steps: mixing carotenoid crystals with ethanol aqueous solution, stirring and dispersing, adding an antioxidant and then removing the solvent, adding perilla seed oil and mixing evenly to obtain a pretreated mixture.

4. The composition according to claim 3, characterized in that The mass ratio of the carotenoid crystals to the ethanol aqueous solution is 1:(3-5).

5. The composition according to claim 3, characterized in that The mass percentage of ethanol in the ethanol aqueous solution is 50-70%.

6. The composition according to claim 3, characterized in that The antioxidant includes any one of ascorbic acid, ascorbyl palmitate, sucrose fatty acid ester, tocopherol, fatty acid ascorbic acid ester, butylated hydroxytoluene, butylated hydroxyanisole, propyl gallic acid or tert-butylhydroxyquinoline, or a combination of at least two thereof.

7. The composition according to claim 3, characterized in that The ethanol residual content in the pretreated carotenoid crystals is less than 10 ppm.

8. The composition according to claim 3, characterized in that The water content of the pretreated carotenoid crystals is 10-30%.

9. The composition according to claim 1, characterized in that The preparation method of the gelled wall material comprises the following steps: dissolving the wall material and carbohydrate to obtain an aqueous solution, and dispersing, stirring and gelling the aqueous solution to obtain the gelled wall material.

10. The composition according to claim 9, characterized in that The mass ratio of the wall material to the carbohydrate is (1-5):

1.

11. The composition according to claim 9, characterized in that The wall material comprises any one or a combination of at least two of sodium starch octenylsuccinate, gum arabic or cellulose derivatives.

12. The composition according to claim 11, characterized in that The wall material is gum arabic.

13. The composition according to claim 9, characterized in that The carbohydrates include any one of sucrose, glucose, glucose syrup, xylose, malto-oligosaccharides, fructo-oligosaccharides or solid corn syrup, or a combination of at least two of them.

14. The composition according to claim 13, characterized in that The carbohydrate is glucose.

15. The composition according to claim 1, characterized in that The one-time embedding includes the steps of mixing, emulsification and drying.

16. The composition according to claim 15, characterized in that The emulsifier used in the emulsification process includes any one of sucrose fatty acid ester, Tween or Span, or a combination of at least two of them.

17. A method for preparing the carotenoid preparation composition according to any one of claims 1 to 16, characterized in that: The preparation method comprises the following steps: (1) mixing carotenoid crystals with an ethanol aqueous solution, stirring and dispersing, adding an antioxidant and removing the solvent, adding perilla seed oil and mixing uniformly to obtain a pretreated mixture; (2) dissolving the wall material and the carbohydrate to obtain an aqueous solution, and dispersing, stirring, and gelling the aqueous solution to obtain a gelled wall material; (3) mixing the pretreated carotenoid crystals with the gelling wall material, emulsifying and drying to obtain a primary encapsulation product; (4) melting the hydrogenated palm oil, mixing it with the primary embedding product, and atomizing it to prepare a composition of the carotenoid preparation; There is no restriction on the order of steps (1) and (2).

18. The preparation method according to claim 17, characterized in that: In step (1), the stirring temperature is 40-50°C and the time is at least 20 minutes.

19. The preparation method according to claim 17, characterized in that The temperature for removing the solvent is 70-80°C.

20. The preparation method according to claim 17, characterized in that The mass percentage of soluble solids in the aqueous solution is 50-70%.

21. The preparation method according to claim 17, characterized in that In step (2), the dispersion temperature is 50-70°C.

22. The preparation method according to claim 17, characterized in that In step (2), the stirring temperature is 80-90°C and the stirring time is 35-50 min.

23. The preparation method according to claim 17, characterized in that The gelation temperature is 60-65° C. and the gelation time is 110-130 min.

24. The preparation method according to claim 17, characterized in that The atomization pressure is 0.2-0.4 MPa, and the temperature of the material during atomization is 13-17°C.

25. The preparation method according to claim 17, characterized in that The preparation method comprises the following steps: (1) Carotenoid crystals are mixed with an ethanol aqueous solution, stirred at 40-50°C for at least 20 min, dispersed, an antioxidant is added, and the solvent is removed at 70-80°C. Perilla seed oil is added and mixed uniformly to obtain a pretreated mixture; (2) dissolving the wall material and carbohydrate to obtain an aqueous solution having a soluble solid content of 50-70% by weight, dispersing the aqueous solution at 50-70° C., stirring at 80-90° C. for 35-50 min, and gelling at 60-65° C. for 110-130 min to obtain a gelled wall material; (3) mixing the pretreated carotenoid with the gelling wall material, emulsifying and drying to obtain a primary encapsulation product; (4) melting hydrogenated palm oil and mixing it with the primary encapsulation product, atomizing the mixture at a pressure of 0.2-0.4 MPa, wherein the temperature of the material during atomization is 13-17° C., to prepare the carotenoid preparation composition; There is no restriction on the order of steps (1) and (2).

26. Use of the carotenoid preparation composition according to any one of claims 1 to 16 in the preparation of food or medicine.

27. Use of the carotenoid preparation composition according to any one of claims 1 to 16 in preparing beverages or health products.

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