Anhydrous astaxanthin emulsion and its preparation method and application

Abstract

The present application relates to astaxanthin emulsion technical field, especially to a kind of anhydrous astaxanthin emulsion and its preparation method and application.The present application provides a kind of preparation method of anhydrous astaxanthin emulsion, comprising the following steps: astaxanthin oil, span, antioxidant and phospholipid first mixing, obtain first emulsion;Tween, glycerol and ethanol second mixing, obtain second emulsion;The first emulsion and second emulsion third mixing, obtain third emulsion;The third emulsion is carried out high pressure homogenization, obtain the anhydrous astaxanthin emulsion;The purity of ethanol is ≥95vol%.The anhydrous astaxanthin emulsion prepared by the preparation method has high stability, good water solubility and high astaxanthin content.

Description

Technical Field

[0001] This invention relates to the field of astaxanthin emulsion technology, and more particularly to an anhydrous astaxanthin emulsion, its preparation method, and its application. Background Technology

[0002] Natural astaxanthin, obtained from Haematococcus pluvialis, is an orange-red ketocarotenoid. It can inhibit lipid oxidation in food, effectively scavenge free radicals in the body, and possesses various biological activities, including enhancing immunity. Therefore, astaxanthin extracted from Haematococcus pluvialis has broad application prospects in food, cosmetics, and skincare products.

[0003] Because natural astaxanthin is a fat-soluble substance, it has extremely poor solubility in water-soluble systems, limiting its application to capsules and powders. Furthermore, astaxanthin has a long-chain, unsaturated, conjugated double-bond structure, making it unstable and prone to isomerization and degradation. Astaxanthin is sensitive to oxygen, sunlight, ultraviolet radiation, and temperature; heat treatment and alkaline conditions can all induce isomerization, significantly restricting its widespread application.

[0004] Currently, there are two methods for storing astaxanthin raw materials: Haematococcus pluvialis powder and Haematococcus pluvialis oil (also known as astaxanthin oil). The latter is an extract of the former and has a viscosity similar to asphalt. Only two dosage forms are popular on the market: solid beverages (microencapsulated astaxanthin or Haematococcus pluvialis powder) and soft capsules (Haematococcus pluvialis oil embedded in gelatin). However, both have significant disadvantages: the former, due to its exposed processing and oxidation, has low potency and is largely abandoned by the market; the latter requires oral digestion and hydrolysis for absorption, thus posing a challenge to consumers' digestive abilities, and also has poor bioavailability and a less than ideal user experience. To address these issues, an increasing number of researchers are studying astaxanthin emulsifiers to attempt to store the astaxanthin raw materials. Currently, common astaxanthin emulsifiers include solvent-based microcapsule encapsulation technology, nanoparticle emulsifier stabilization technology, and ethyl cellulose-whey protein composite systems. However, due to the special physicochemical properties of astaxanthin, astaxanthin emulsions may have poor water solubility, precipitation, stratification, or low astaxanthin content, and have not yet successfully overcome the bottlenecks and achieved industrialization.

[0005] Water is an indispensable basic ingredient in emulsions and the best solvent in nature. As the most abundant ingredient in emulsions, water typically accounts for 60% to 80%, or even higher. However, the high dissolved oxygen content in water (6-8 mg / L) is extremely detrimental to easily oxidized, unstable, or easily degraded active ingredients, especially antioxidants. Adding oxygen-containing water to antioxidant emulsions will inevitably oxidize astaxanthin, reducing its potency and affecting its function. Although dissolved oxygen can be removed or water purified through physical or chemical methods, this requires significant energy expenditure or the use of large amounts of chemical solvents, and further removal is necessary afterward, hindering expansion in the food market. Currently, easily oxidized antioxidants or peptides and plant extracts that require specific pH ranges to be effective typically require chemical modification, microencapsulation, or other process improvements, or even be made directly into capsules without emulsification. Among them, the safety risks caused by the byproducts remaining from chemical modification should not be underestimated; while process improvements such as microencapsulation increase water solubility, they cannot prevent oxidation and also increase the failure rate and production cost of product development, so their application prospects are not promising.

[0006] In summary, anhydrous emulsion systems present two main challenges: 1. Replacing water, the best natural solvent, with polyols places higher demands on the solubility of active ingredients; 2. Unlike traditional water-based or cream products, replacing water with polyols presents greater challenges to product stability. Ensuring the stability and bioavailability of anhydrous or low-water emulsion systems for astaxanthin remains a significant challenge. Summary of the Invention

[0007] In view of this, the purpose of the present invention is to provide an anhydrous astaxanthin emulsion, its preparation method and application, wherein the anhydrous astaxanthin emulsion prepared by the preparation method has high stability, good water solubility and high astaxanthin content.

[0008] To achieve the above-mentioned objectives, the present invention provides the following technical solution:

[0009] This invention provides a method for preparing anhydrous astaxanthin emulsion, comprising the following steps:

[0010] The astaxanthin oil, Span, antioxidants and phospholipids are first mixed to obtain the first emulsion;

[0011] Tween, glycerol and ethanol are mixed again to obtain a second emulsion;

[0012] The first emulsion and the second emulsion are mixed to obtain a third emulsion;

[0013] The third emulsion was homogenized under high pressure to obtain the anhydrous astaxanthin emulsion.

[0014] The purity of the ethanol is ≥95 vol.

[0015] Preferably, the mass ratio of the astaxanthin oil to the Span is 1:(0.1~3), and the mass percentage of astaxanthin in the astaxanthin oil is 5%~10%.

[0016] The mass ratio of astaxanthin oil to phospholipids is 1:(0.1~5).

[0017] The mass ratio of astaxanthin oil to antioxidant is 1:(0.1~15).

[0018] Preferably, the spitting includes one or more of spitting 20, spitting 40, spitting 60 and spitting 80;

[0019] The antioxidants include one or more of the following: vitamin E, ascorbyl palmitate, lycopene, lutein, beta-carotene, grape seed oil extract, coenzyme Q10, sulforaphane, and tea polyphenols.

[0020] The phospholipids include one or more of phosphatidylcholine, choline phospholipids, lecithin, soybean phospholipids, L-α-glucosinolate choline, and hydrolyzed egg yolk powder.

[0021] Preferably, the mass ratio of the tween to glycerol is 5:1 to 1:5;

[0022] The mass ratio of Tween to ethanol is 1:(0.1~20).

[0023] Preferably, the Tween includes one or more of Tween 80, Tween 60, Tween 40, and Tween 20.

[0024] Preferably, the mass ratio of the first emulsion to the second emulsion is 1:(0.5~10).

[0025] Preferably, after obtaining the third emulsion, the process further includes mixing the third emulsion, the suspending agent, and the ion chelating agent, and then performing the high-pressure homogenization.

[0026] The mass ratio of the third emulsion to the total mass of the suspending agent and the ion chelating agent is (100~1000):1;

[0027] The mass ratio of the suspending agent to the ion chelating agent is 1:(0.5-2).

[0028] Preferably, the suspending agent comprises one or more of the following: gelatinous substances, cellulose-modified materials, proteins, and degradation product peptides;

[0029] The gum-like substances include one or more of gum arabic, polyvinylpyrrolidone, xanthan gum, Indian gum, guar gum, and gelatin;

[0030] The cellulose-modified material includes one or more of sodium carboxymethyl cellulose, hydroxypropyl methyl cellulose, sodium carboxymethyl cellulose, and cellulosic ethanol;

[0031] The protein includes one or more of soy protein, corn protein, and albumin;

[0032] The degradation product peptides include one or more of the following: hydrolyzed soybean protein, corn protein, hydrolyzed egg protein, and wheat oligopeptides.

[0033] The ion chelating agent includes one or more of EDTA-Na2, sodium tripolyphosphate, and citric acid.

[0034] The present invention also provides an anhydrous astaxanthin emulsion prepared by the preparation method described above, wherein the water content of the anhydrous astaxanthin emulsion is ≤5wt% and the astaxanthin content in the anhydrous astaxanthin emulsion is ≥10mg / mL.

[0035] The present invention also provides the application of the anhydrous astaxanthin emulsion described above in cosmetics or food.

[0036] This invention provides a method for preparing anhydrous astaxanthin emulsion, comprising the following steps: firstly mixing astaxanthin oil, Span, an antioxidant, and phospholipids to obtain a first emulsion; secondly mixing Tween, glycerol, and ethanol to obtain a second emulsion; thirdly mixing the first and second emulsions to obtain a third emulsion; and homogenizing the third emulsion under high pressure to obtain the anhydrous astaxanthin emulsion; wherein the purity of the ethanol is ≥95 vol%. The preparation method of this invention uses a composite emulsifier composed of Tween, Span, and phospholipids, which are both hydrophilic and lipophilic, to prepare anhydrous astaxanthin emulsion. This not only provides the advantages of a single surfactant but also leverages the synergistic effect of various emulsifiers, resulting in better emulsification and stability. Compared to commonly used anionic emulsifiers, this method offers better emulsification but less stability, and is prone to demulsification and rancidity over time. Therefore, the composite emulsifier described in this invention can significantly reduce the surface tension between water and oil, enabling them to form a stable emulsion system, thereby improving emulsion stability and freeze-thawability. Simultaneously, by using a combination of multiple emulsifiers, the HLB of the composite emulsifier can be adjusted to better match the emulsified object, resulting in excellent stability and preventing emulsion system stratification, precipitation, or coagulation, thus ensuring product quality and performance. Even in ethanol-based emulsions, where instability is more likely, the composite emulsifier described in this invention can increase the solubility of oily substances in ethanol, improving product stability, solubility, and effectiveness. Ultimately, this results in astaxanthin emulsions with high potency, good stability, and long shelf life. This is especially true for emulsions using 95° or higher (purity ≥95 vol%) ethanol containing trace amounts of water as the water-based base, further highlighting its stability and high potency. Because all emulsifiers used are food-grade, their dilution ratio ensures they remain within safe usage limits during application, and the astaxanthin content is also within the effective dosage range. Therefore, their use in the food and cosmetic fields can fully leverage the antioxidant and free radical scavenging functions of astaxanthin. Furthermore, the preparation method is simple, easy to implement, environmentally friendly, allows for continuous production, and boasts high efficiency. Attached Figure Description

[0037] Figure 1 The image shows a microscopic view (×200) of the astaxanthin concentrated emulsion prepared in Example 1 of this invention.

[0038] Figure 2 This is a microscopic image of the astaxanthin concentrated emulsion prepared in Comparative Example 7. Detailed Implementation

[0039] This invention provides a method for preparing anhydrous astaxanthin emulsion, comprising the following steps:

[0040] The astaxanthin oil, Span, antioxidants and phospholipids are first mixed to obtain the first emulsion;

[0041] Tween, glycerol and ethanol are mixed again to obtain a second emulsion;

[0042] The first emulsion and the second emulsion are mixed to obtain a third emulsion;

[0043] The third emulsion was homogenized under high pressure to obtain the anhydrous astaxanthin emulsion.

[0044] The purity of the ethanol is ≥95 vol.

[0045] In this invention, unless otherwise specified, all raw materials used in the preparation are commercially available products well known to those skilled in the art.

[0046] In this invention, the anhydrous astaxanthin emulsion can be understood as having no additional water added, and except for ethanol which contains <5 vol% water (or does not contain water), the other raw materials do not contain water.

[0047] The present invention first mixes astaxanthin oil, Span, antioxidant and phospholipid to obtain a first emulsion.

[0048] In this invention, the Span preferably includes one or more of Span 20, Span 40, Span 60, and Span 80, more preferably including Span 80. When the Span is two or more of the above-mentioned specific selections, this invention does not have any special limitation on the ratio of the above-mentioned specific substances, and they can be mixed in any ratio. In an embodiment of this invention, the Span can be Span 80 (sorbitan glyceride).

[0049] In this invention, the mass ratio of astaxanthin oil to Span is preferably 1:(0.1~3), more preferably 1:(0.5~1). In this invention, the mass percentage content of astaxanthin in the astaxanthin oil is preferably 5%~10%. In an embodiment of this invention, the mass ratio of astaxanthin oil to Span can be 1:1. In an embodiment of this invention, the mass percentage content of astaxanthin in the astaxanthin oil can be 10%.

[0050] In this invention, the antioxidant preferably includes one or more of vitamin E, ascorbyl palmitate, lycopene, lutein, β-carotene, grape seed oil extract, coenzyme Q10, sulforaphane, and tea polyphenols, more preferably vitamin E. When the antioxidant is two or more of the above-mentioned specific selections, this invention does not impose any special limitation on the ratio of the above-mentioned substances, and they can be mixed in any ratio. In an embodiment of this invention, the antioxidant is vitamin E.

[0051] In this invention, the mass ratio of astaxanthin oil to antioxidant is preferably 1:(0.1~15), more preferably 1:(0.2~1), and most preferably 1:0.5. In embodiments of this invention, the mass ratio of astaxanthin oil to antioxidant can be 1:0.2 or 1:0.5.

[0052] In this invention, the phospholipids preferably include one or more of phosphatidylcholine, choline phospholipids, lecithin, soybean phospholipids, L-α-glycine phosphocholine, and hydrolyzed egg yolk powder, more preferably soybean phospholipids. When the phospholipids are two or more of the above-mentioned specific selections, this invention does not impose any special limitation on the ratio of the above-mentioned specific substances, and they can be mixed in any ratio. In the embodiments of this invention, the phospholipids can be soybean phospholipids.

[0053] In this invention, the mass ratio of astaxanthin oil to phospholipids is preferably 1:(0.1~5), more preferably 1:(2~5). In embodiments of this invention, the mass ratio of astaxanthin to phospholipids can be 1:5 or 1:4.

[0054] In this invention, the role of the Span is to emulsify and disperse astaxanthin oil, the role of the antioxidant is to protect astaxanthin from oxidation and maintain its high efficiency and stability, and the role of the phospholipid is to emulsify.

[0055] In this invention, the first mixing is preferably carried out under heating and stirring conditions. The heating temperature is preferably 55-65°C, more preferably 58-62°C; the stirring speed is preferably 30-100 rpm, more preferably 40-80 rpm; and the first mixing time is preferably 10-30 min, more preferably 15-25 min. In an embodiment of this invention, the heating temperature can be 60°C, the stirring speed can be 50 rpm, and the first mixing time can be 30 min.

[0056] The preparation method of the present invention further includes mixing Tween, glycerol and ethanol to obtain a second emulsion.

[0057] In this invention, the Tween preferably includes one or more of Tween 80, Tween 60, Tween 40, and Tween 20, and more preferably includes Tween 80. When the Tween is two or more of the above-mentioned specific selections, this invention does not impose any special limitation on the ratio of the above-mentioned specific substances, and they can be mixed in any ratio. In an embodiment of this invention, the Tween can be Tween 80 (polysorbate-80).

[0058] In this invention, the purity of the glycerol is preferably ≥99%.

[0059] In this invention, the mass ratio of Tween to glycerol is preferably 5:1 to 1:5, more preferably 4:1 to 1:4. In embodiments of this invention, the mass ratio of Tween to glycerol can be 2:1 or 2:1.5.

[0060] In this invention, the mass ratio of Tween to ethanol is preferably 1:(0.1~20), more preferably 1:(0.2~10), and most preferably 1:(0.5~8). In embodiments of this invention, the mass ratio of Tween to ethanol can be 1:4 or 1:5.

[0061] In this invention, Tween acts as an emulsifier, while glycerol and ethanol replace the water base in the emulsion and promote the dissolution of astaxanthin oil.

[0062] In this invention, the second mixing is preferably carried out under heating and stirring conditions. The heating temperature is preferably 55-65°C, more preferably 58-62°C; the stirring speed is preferably 30-100 rpm, more preferably 40-80 rpm; and the second mixing time is preferably 10-30 min, more preferably 15-25 min. In an embodiment of this invention, the heating temperature can be 60°C, the stirring speed can be 50 rpm, and the second mixing time can be 10 min.

[0063] After obtaining the first emulsion and the second emulsion, the present invention further includes mixing the first emulsion and the second emulsion to obtain a third emulsion.

[0064] In this invention, the mass ratio of the first emulsion to the second emulsion is preferably 1:(0.5~10), more preferably 1:(2~5). In embodiments of this invention, the mass ratio of the first emulsion to the second emulsion can be 1:0.5 or 1:4.

[0065] In this invention, the third mixing is preferably carried out under heating and stirring conditions. The heating temperature is preferably 55-60°C, more preferably 56-59°C. The stirring preferably includes a first stirring and a second stirring performed sequentially. The rotation speed of the first stirring is preferably 30-100 rpm, more preferably 40-80 rpm. The stirring time of the first stirring is preferably 5-60 min, more preferably 10-30 min. The rotation speed of the second stirring is preferably 10-50 rpm, more preferably 30 rpm. The stirring time of the second stirring is preferably 10-60 min, more preferably 30 min. In an embodiment of this invention, the rotation speed of the first stirring can be 30 rpm and the stirring time can be 30 min, and the rotation speed of the second stirring can be 30 rpm and the stirring time can be 30 min.

[0066] After obtaining the third emulsion, the present invention performs high-pressure homogenization on the third emulsion to obtain the anhydrous astaxanthin emulsion.

[0067] In this invention, the pressure of the high-pressure homogenization is preferably 15 / 65MPa~30 / 150MPa, the time is preferably 10~30min, and the temperature is preferably 55℃.

[0068] After the high-pressure homogenization is completed, the present invention preferably includes cooling. The present invention does not have any special limitations on the cooling process, and any process known to those skilled in the art can be used.

[0069] Alternatively, after obtaining the third emulsion, the present invention preferably further includes mixing the third emulsion, the suspending agent, and the ion chelating agent, and then performing high-pressure homogenization.

[0070] In this invention, the mixing is preferably a mixture of the third emulsion and a mixture of the suspending agent and the ion chelating agent; the mixture of the suspending agent and the ion chelating agent is preferably obtained by mixing the suspending agent and the ion chelating agent. In this invention, the mass ratio of the third emulsion to the total mass of the suspending agent and the ion chelating agent is preferably (100~1000):1, more preferably (200~500):1; the mass ratio of the suspending agent to the ion chelating agent is preferably 1:(0.5~2), more preferably 1:(1~2). In embodiments of this invention, the mass ratio of the third emulsion to the total mass of the suspending agent and the ion chelating agent can be 500:1 or 800:1, and the mass ratio of the suspending agent to the ion chelating agent can be 1:1 or 1:1.2.

[0071] In this invention, the suspending agent preferably includes one or more of the following: gum substances, cellulose-modified materials, proteins, and degradation product peptides; the gum substances preferably include one or more of the following: gum arabic, polyvinylpyrrolidone, xanthan gum, Indian gum, guar gum, and gelatin; the cellulose-modified materials preferably include one or more of the following: sodium carboxymethyl cellulose, hydroxypropyl methylcellulose, sodium carboxymethyl cellulose, and cellulosic ethanol; the proteins preferably include one or more of the following: soy protein, corn protein, and albumin; the degradation product peptides preferably include one or more of the following: hydrolyzed soy protein, corn protein, hydrolyzed egg protein, and wheat oligopeptides; the suspending agent more preferably includes polyvinylpyrrolidone; when the suspending agent is two or more of the above-mentioned specific selections, this invention does not have any special limitation on the ratio of the above-mentioned specific substances, and they can be mixed in any ratio.

[0072] In this invention, the ion chelating agent preferably includes one or more of EDTA-Na2, sodium tripolyphosphate and citric acid, more preferably EDTA-Na2; when the ion chelating agent is two or more of the above-mentioned specific selections, this invention does not have any special limitation on the ratio of the above-mentioned specific substances, and they can be mixed in any ratio.

[0073] In this invention, the suspending agent can further prevent astaxanthin from precipitating or dissolving, and the ion chelating agent can protect and stabilize astaxanthin by chelating metal ions.

[0074] The present invention does not impose any special limitations on the mixing process; any process known to those skilled in the art can be used.

[0075] In this invention, the mixing of the third emulsion with the mixture of the suspending agent and the ion chelating agent is preferably carried out by adding the mixture of the suspending agent and the ion chelating agent to the third emulsion. In this invention, the addition rate of the mixture of the suspending agent and the ion chelating agent is preferably 0.5~10 g / min, more preferably 5~10 g / min. In an embodiment of this invention, the addition rate of the mixture of the suspending agent and the ion chelating agent can be 5 g / min.

[0076] In this invention, the pressure of the high-pressure homogenization is preferably 15 / 65MPa~30 / 150MPa, the time is preferably 30-60min, and the temperature is preferably 50~60℃.

[0077] The present invention also provides an anhydrous astaxanthin emulsion prepared by the preparation method described above, wherein the water content of the anhydrous astaxanthin emulsion is ≤5wt% and the astaxanthin content in the anhydrous astaxanthin emulsion is ≥10mg / mL.

[0078] This invention also provides the application of the anhydrous astaxanthin emulsion described above in cosmetics or food. In this invention, the cosmetics preferably include emulsions, facial mask liquids, or serums; the food preferably includes concentrates, beverages, or oral liquids. This invention does not impose any special limitations on the method of application; any method well-known to those skilled in the art can be used.

[0079] The technical solutions of this invention will be clearly and completely described below with reference to the embodiments thereof. Obviously, the described embodiments are only a part of the embodiments of this invention, and not all of them. All other embodiments obtained by those skilled in the art based on the embodiments of this invention without creative effort are within the scope of protection of this invention.

[0080] Example 1

[0081] According to the mass ratio of 1:1:0.2:5, astaxanthin oil (astaxanthin content of 10%), Span 80, vitamin E and soybean lecithin are mixed and stirred in a water bath at 60°C for 30 minutes (stirring speed of 50 rpm) until the mixture is uniform, to obtain the first emulsion.

[0082] Tween 80, glycerol and anhydrous ethanol were mixed in a mass ratio of 2:1:8 and stirred at 60°C (30 rpm) for 30 min to obtain the second emulsion.

[0083] The first emulsion and the second emulsion were mixed at a mass ratio of 1:0.5. The mixture was stirred at 30 rpm for 10 minutes at 60°C, and then stirred at 2800 rpm for 10 minutes until it was uniformly mixed. The mixture was then cooled to room temperature to obtain the third emulsion.

[0084] Polyvinylpyrrolidone and EDTA-Na2 were mixed evenly at a mass ratio of 1:1 to obtain a mixture.

[0085] The mixture was slowly added to the third emulsion at a mass ratio of 1:500 (addition rate of 1 mL / min), and high-pressure homogenization was performed (pressure of 20 / 150 MPa, time of 20 min, temperature of 60 °C) to obtain anhydrous astaxanthin emulsion (astaxanthin content of 1.48 ± 0.15%, water content of 3.8%).

[0086] Figure 1 Micrograph (×200) of the astaxanthin concentrate emulsion prepared in Example 1, from which... Figure 1 It can be seen that the astaxanthin concentrated emulsion is stable and uniform;

[0087] The anhydrous astaxanthin emulsion was stored at room temperature, protected from light, radiation, and ultraviolet irradiation. The astaxanthin content of the anhydrous astaxanthin emulsion was tested according to the United States Food Chemicals Codex (8th Edition) (FCC8) using HPLC. The test results are shown in Table 1.

[0088] Table 1. Astaxanthin content (g / 100g) of the anhydrous astaxanthin emulsion after storage for different number of days.

[0089]

[0090] Example 2

[0091] According to the mass ratio of 1:1:0.5:4, astaxanthin oil (astaxanthin content of 10%), Span 80, vitamin E and hydrolyzed egg yolk powder are mixed and stirred in a water bath at 55°C for 30 minutes (stirring speed of 28 rpm) until the mixture is uniform, to obtain the first emulsion.

[0092] Tween 80, glycerol and anhydrous ethanol were mixed in a mass ratio of 2:1.5:10 and stirred at 55°C (28 rpm) for 20 min to obtain the second emulsion.

[0093] The first emulsion and the second emulsion were mixed at a mass ratio of 1:4. The mixture was stirred at 28 rpm for 20 minutes at 55°C, and then stirred at 2800 rpm for 30 minutes until it was uniformly mixed. The mixture was then cooled to room temperature to obtain the third emulsion.

[0094] Polyvinylpyrrolidone and EDTA-Na2 were mixed evenly at a mass ratio of 1:1.2 to obtain a mixture.

[0095] The mixture was slowly added to the third emulsion at a mass ratio of 1:800 (addition rate of 5 mL / min), and high-pressure homogenization was performed (pressure of 20 / 150 MPa, time of 15 min, temperature of 55 °C) to obtain anhydrous astaxanthin emulsion (astaxanthin content of 1.52 ± 0.12%, water content of 3.15%).

[0096] The anhydrous astaxanthin emulsion was stored at room temperature, protected from light, radiation, and ultraviolet irradiation. The astaxanthin content of the anhydrous astaxanthin emulsion was tested by HPLC according to the United States Food Chemicals Codex (8th Edition) (FCC8). The test results are shown in Table 2.

[0097] Table 2 shows the astaxanthin content (g / 100g) of the anhydrous astaxanthin emulsion after storage for different numbers of days.

[0098]

[0099] Comparative Example 1

[0100] Referring to Example 1, the difference is that the first emulsion does not contain soybean lecithin, resulting in an anhydrous astaxanthin emulsion (astaxanthin content is 0.55%, water content is 4.4%).

[0101] The anhydrous astaxanthin emulsion was stored at room temperature, protected from light, radiation, and ultraviolet irradiation. The astaxanthin content of the anhydrous astaxanthin emulsion was tested by HPLC according to the United States Food Chemicals Codex (8th Edition) (FCC8). The test results are shown in Table 3.

[0102] Table 3. Astaxanthin content (g / 100g) of the anhydrous astaxanthin emulsion after storage for different number of days.

[0103]

[0104] Comparative Example 2

[0105] Referring to Example 1, the difference is that the first emulsion does not include Span 80, resulting in an anhydrous astaxanthin emulsion (astaxanthin content is 0.76%, water content is 3.6%).

[0106] The anhydrous astaxanthin emulsion was stored at room temperature, protected from light, radiation, and ultraviolet irradiation. The astaxanthin content of the anhydrous astaxanthin emulsion was tested by HPLC according to the United States Food Chemicals Codex (8th Edition) (FCC8). The test results are shown in Table 4.

[0107] Table 4 shows the astaxanthin content (g / 100g) of the anhydrous astaxanthin emulsion after storage for different number of days.

[0108]

[0109] Comparative Example 3

[0110] Referring to Example 1, the difference is that the second emulsion does not include Tween 80, resulting in an anhydrous astaxanthin emulsion (astaxanthin content is 0.44%, water content is 0.35%).

[0111] The anhydrous astaxanthin emulsion was stored at room temperature, protected from light, radiation, and ultraviolet irradiation. The astaxanthin content of the anhydrous astaxanthin emulsion was tested by HPLC according to the United States Food Chemicals Codex (8th Edition) (FCC8). The test results are shown in Table 5.

[0112] Table 5. Astaxanthin content (g / 100g) of the anhydrous astaxanthin emulsion after storage for different number of days.

[0113]

[0114] Comparative Examples 4-6

[0115] Referring to Example 1, the difference is that the Span 80 is replaced with Span 60 (Comparative Example 4), or the soybean lecithin is replaced with hydrolyzed egg yolk powder (Comparative Example 5), or the Tween 80 is replaced with Tween 20 (Comparative Example 6).

[0116] The anhydrous astaxanthin emulsion was stored at room temperature, protected from light, radiation, and ultraviolet irradiation. The astaxanthin content of the anhydrous astaxanthin emulsion was tested by HPLC according to the United States Food Chemicals Codex (8th Edition) (FCC8). The test results are shown in Table 6.

[0117] Table 6. Astaxanthin content (g / 100g) of the anhydrous astaxanthin emulsion after storage for different number of days.

[0118]

[0119] Comparative Example 7

[0120] Step 1: Mix Tween 80 and phospholipid Pc35 at a mass ratio of 3.6:1, heat in a water bath to 50°C, and magnetically stir for 8 minutes until fully dissolved and homogeneous to obtain a composite emulsifier. Step 2: Mix the composite emulsifier and propylene glycol at a mass ratio of 5.3:1, heat in a water bath to 50°C, and magnetically stir for 3 minutes until fully mixed to obtain a composite emulsion stabilizer; the purity of the propylene glycol is above 99%. Step 3: Mix the composite emulsion stabilizer and astaxanthin oil with an astaxanthin content of 10% at a mass ratio of 5.25:1, heat in a water bath to 45°C, and magnetically stir for 1 minute until fully mixed. Cool to room temperature, and homogenize once under high pressure at a pressure of 20 / 100 MPa to obtain a hydrophilic astaxanthin emulsion dispersion oil.

[0121] Figure 2 This is a microscopic image (×200) of the astaxanthin emulsion described in Comparative Example 7, created by... Figure 2 It is known that the astaxanthin emulsion is uneven, thick, and prone to sedimentation or floating. Furthermore, according to page 22 of the latest national standard GB 2760-2024, the National Food Safety Standard for the Use of Food Additives, propylene glycol is only permitted for use in pastries and flour products, not in emulsions, and the maximum permitted usage is only 3.0 g / kg (in pastries). The propylene glycol in this comparative example accounts for 14% of the mass of the hydrophilic astaxanthin emulsion dispersion oil, which does not comply with GB 2760-2024.

[0122] Application Example 1

[0123] Application in oral liquids:

[0124] The anhydrous astaxanthin emulsion described in Example 2 was mixed with deionized water at a volume ratio of 1:150 to obtain a stable, clear, and semi-transparent water-soluble astaxanthin emulsion (the water-soluble astaxanthin emulsion does not separate into layers or cling to the cup wall and can be consumed directly).

[0125] Application Example 2

[0126] Application in serums:

[0127] At a temperature of 55°C, the anhydrous astaxanthin emulsion described in Example 2 and 95% ethanol were mixed at a volume ratio of 1:0.5 and then filled into ampoules pre-blown with nitrogen to obtain an essence (a uniform red liquid; when using, simply open the ampoule and apply directly to the skin).

[0128] Application Example 3

[0129] Application of astaxanthin in topical facial masks:

[0130] At a temperature of 50°C, the anhydrous astaxanthin emulsion and 95% ethanol described in Example 2 were mixed at a volume ratio of 1:15 to obtain an astaxanthin facial mask liquid (in a red, uniform liquid state). The astaxanthin facial mask liquid was then filled into a pre-blown nitrogen- or vacuum-sealed facial mask bag. When using the mask, the astaxanthin facial mask liquid was poured out, mixed with other facial mask liquids, and then soaked into a facial mask sheet before use.

[0131] The above description is merely a preferred embodiment of the present invention and is not intended to limit the present invention in any way. It should be noted that those skilled in the art can make various improvements and modifications without departing from the principles of the present invention, and these improvements and modifications should also be considered within the scope of protection of the present invention.

Claims

1. A method for preparing anhydrous astaxanthin emulsion, characterized in that, It consists of the following steps: The astaxanthin oil, Span, antioxidants and phospholipids are first mixed to obtain the first emulsion; Tween, glycerol and anhydrous ethanol are mixed in a second mixture to obtain a second emulsion; The first emulsion and the second emulsion are mixed to obtain a third emulsion; The third emulsion was homogenized under high pressure to obtain the anhydrous astaxanthin emulsion. The mass ratio of Tween to glycerol is 2:(1~1.5); the mass ratio of Tween to anhydrous ethanol is 1:(4~20). The mass ratio of the first emulsion to the second emulsion is 1:(0.5~10).

2. The preparation method according to claim 1, characterized in that, The mass ratio of the astaxanthin oil to the Span is 1:(0.1~3), and the mass percentage of astaxanthin in the astaxanthin oil is 5%~10%. The mass ratio of astaxanthin oil to phospholipids is 1:(0.1~5). The mass ratio of astaxanthin oil to antioxidant is 1:(0.1~15).

3. The preparation method according to claim 2, characterized in that, The spoofing includes one or more of spoofing 20, spoofing 40, spoofing 60 and spoofing 80; The antioxidants include one or more of the following: vitamin E, ascorbyl palmitate, lycopene, lutein, beta-carotene, grape seed oil extract, coenzyme Q10, sulforaphane, and tea polyphenols. The phospholipids include one or more of phosphatidylcholine, lecithin, soybean phospholipids, and L-α-glucosinolates.

4. The preparation method according to claim 1, characterized in that, The Tween includes one or more of Tween 80, Tween 60, Tween 40, and Tween 20.

5. The preparation method according to claim 1, characterized in that, After obtaining the third emulsion, the process further includes mixing the third emulsion, suspending agent, and ion chelating agent, and then performing the high-pressure homogenization. The mass ratio of the third emulsion to the total mass of the suspending agent and the ion chelating agent is (100~1000):1; The mass ratio of the suspending agent to the ion chelating agent is 1:(0.5-2).

6. The preparation method according to claim 5, characterized in that, The suspending agent includes one or more of the following: gelatinous substances, cellulose-modified materials, proteins, and degradation product peptides; The gum-like substances include one or more of gum arabic, xanthan gum, gum arabic, guar gum, and gelatin; The cellulose-modified material includes one or more of hydroxypropyl methylcellulose and sodium carboxymethyl cellulose; The protein includes one or more of soy protein, corn protein, and albumin; The degradation product peptides include one or more of soybean hydrolysate, egg hydrolysate and wheat oligopeptides. The ion chelating agent includes one or more of EDTA-2Na, sodium tripolyphosphate, and citric acid.

7. The use of the anhydrous astaxanthin emulsion prepared by the preparation method according to any one of claims 1 to 6 in cosmetics or food.

Images