Color capsules containing anthocyanins and a method for production thereof

The biphasic emulsion-in-emulsion structure with anthocyanins from purple basil leaves, encapsulated in a biopolymer gel, addresses absorption and stability issues, enhancing bioaccessibility and stability for use in food, cosmetics, and pharmaceuticals.

WO2026015105A1PCT designated stage Publication Date: 2026-01-15YILDIZ TEKNIK UNIVERSITESI DONER SERMAYE ISLETME MUD +1
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Patent Information

Application Number
PCT/TR2024/051551
Authority / Receiving Office
WO · WO
Patent Type
Applications
Current Assignee / Owner
Filing Date
2024-12-12
Publication Date
2026-01-15

AI Technical Summary

Technical Problem

Existing encapsulation systems for anthocyanins fail to effectively regulate their absorption in the body and maintain stability against external factors, leading to undesirable color changes and limited bioaccessibility.

Method used

A biphasic emulsion-in-emulsion (E/E) structure is created using an anthocyanin extract from purple basil leaves, encapsulated in a biopolymer-based gel-form (emulgel) through electrospraying, with specific parameters for extraction, mixing, and electrospraying processes to enhance bioaccessibility and stability.

Benefits of technology

The emulgel capsules provide increased bioaccessibility and stability of anthocyanins, extending shelf life and preserving color and antioxidant properties, suitable for use in food, cosmetics, and pharmaceutical products.

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Abstract

The invention is a color capsule suitable for use in food products, comprising a primary emulsion emulsified in a biopolymer-based and gel-form secondary emulsion, and an anthocyanin extract emulsified in the primary emulsion. The invention also describes a method for the production of the color capsules of the invention, comprising the process steps of obtaining an anthocyanin extract from plant raw materials (a), emulsifying the anthocyanin extract in a primary emulsion (b), emulsifying the primary emulsion in a biopolymer-based secondary emulsion in order to obtain a biphasic emulsion (c), and spraying the biphasic emulsion into a salt bath using the electrospraying technique in order to form biphasic emulsion-based gel-form capsules (d).
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Description

[0001] DESCRIPTION

[0002] COLOR CAPSULES CONTAINING ANTHOCYANINS AND A METHOD FOR PRODUCTION THEREOF

[0003] Technical Field of the Invention

[0004] The present invention relates to hybrid emulgel capsules with increased bioaccessibility of anthocyanins, which are suitable for use mainly in the food, cosmetics and pharmaceutical industries, and a method for production thereof.

[0005] Background of the Invention

[0006] Especially in the food and cosmetic industries, various colorants are used to increase the attractiveness and appetizingness of the products. Anthocyanins are found especially in red, blue or purple plants, fruits and vegetables, which also give their colors to the products in which they are used. They mainly consist of an aglycone (anthocyanidin) structure connected to a sugar molecule. This structure can change color depending on the pH level of the plant. The color of anthocyanins varies depending on the pH level of the cell. They turn red in acidic environments, purple in neutral environments, and blue in basic environments. Sources of anthocyanins include blueberries, raspberries, blackberries, cherries, strawberries, grapes, plums, red cabbage, eggplant, purple carrots, red onions, purple corn, and black rice.

[0007] On the other hand, the stability of these bioactive components is affected by various factors such as pH, storage temperature, chemical structure, concentration, light, oxygen, solvents, presence of enzymes, proteins, and metallic ions. Therefore, when the raw materials containing anthocyanins or extracts containing anthocyanins are used directly in food products, undesirable color changes may occur in the product, and the absorption of anthocyanins in the body may not be at the desired level, i.e., their bioaccessibility may be limited.

[0008] Encapsulation applications are known in the art to solve this problem and to increase the stability of anthocyanins. For example, TR2021 / 013805 discloses a chocolate containing anthocyanin that is encapsulated with chitosan polymer nanoparticles, and a production method for obtaining same. The method proposed therein comprises the steps of obtaining an extract from purple fruits and / or vegetables, encapsulating the extract with chitosan polymer and mixing anthocyanin-containing capsules with cocoa and cocoa butter.

[0009] In view of the applications in the art to increase the stability of anthocyanins, it has been found that there is still a need for more effective encapsulation systems that allow the regulation of the absorption of anthocyanin in the body, and accordingly for anthocyanincontaining capsules with increased bioaccessibility.

[0010] Objects of the Invention

[0011] The main object of the invention is to provide solutions to the above-mentioned problems in the prior art.

[0012] Another object of the invention is to obtain anthocyanin-loaded capsules in which anthocyanins are effectively isolated from the external environment.

[0013] Another object of the invention is to obtain color capsules with increased bioaccessibility of anthocyanins.

[0014] Another object of the invention is to obtain hybrid color capsules in which anthocyanins are emulsified in an emulsion-in-emulsion (E / E) form (in a biphasic form).

[0015] Another object of the invention is to obtain color capsules in which anthocyanins are constrained in an emulgel structure.

[0016] Another object of the invention is to obtain color capsules loaded with anthocyanins from purple basil leaves (Ocimum basilicum L).

[0017] Another object of the invention is to propose a method for obtaining anthocyanin-loaded and emulgel form capsules.

[0018] Another object of the invention is to propose a method comprising obtaining an anthocyanin extract from purple basil leaves in powder form.

[0019] Another object of the invention is to propose a method comprising biphasic emulsification of the anthocyanin extract.

[0020] Another object of the invention is to propose a method wherein biphasic emulsions containing an anthocyanin extract are encapsulated by electrospraying. Another object of the invention is to propose a method wherein the anthocyanin extract is encapsulated in a biphasic emulsion in gel form.

[0021] Still another object of the invention is to propose a method that allows an effective isolation of anthocyanins from the external environment, thus increasing their bioaccessibility, while extending their shelf life by increasing their resistance against external factors such as storage temperature, light, pH, and thus preserving their color and antioxidant properties.

[0022] Summary of the Invention

[0023] The invention is a color capsule suitable for use in food products, comprising a primary emulsion emulsified in a biopolymer-based and gel-form secondary emulsion, and an anthocyanin extract emulsified in the primary emulsion. In other words, the color capsule of the invention comprises the anthocyanin extract in a biphasic emulsified form.

[0024] According to a preferred embodiment of the invention, the anthocyanin extract is made from purple basil leaves.

[0025] According to the preferred embodiment of the invention, said primary emulsion comprises an oil phase and a water phase containing the anthocyanin extract emulsified in the said oil phase. Accordingly, in an embodiment, said secondary emulsion comprises a biopolymer solution as well as the primary emulsion emulsified in the said biopolymer solution.

[0026] The invention also describes a method for producing the color capsules suitable for use in food products. The method of the invention comprises the following main steps: a. Obtaining an anthocyanin extract from plant raw materials b. Emulsifying the anthocyanin extract in a primary emulsion c. Emulsifying the primary emulsion in a biopolymer-based secondary emulsion in order to obtain a biphasic emulsion d. Forming biphasic emulsion-based gel-form (emulgel) capsules by spraying the biphasic emulsion into a salt bath using an electrospraying technique

[0027] Detailed Description of the Invention The invention describes a color capsule prepared using plant raw materials, in particular those containing anthocyanin. Said plant raw materials refer to any part of the plants, including the fruits.

[0028] According to an optional embodiment of the invention, the color capsule of the invention comprises an anthocyanin extract obtained from purple basil leaves Ocimum basilicum L). Especially those with red or purple leaves are rich in anthocyanins. Anthocyanins are pigments from the flavonoid class that occur naturally in plants and give them their red, purple and blue colors. Therefore, the color capsules of the invention also have a blue, purple or red hue, though varying depending on the color of the purple basil leaves used.

[0029] Since the antioxidant properties of anthocyanins are preserved in the invention, in addition to their coloring properties, it is possible for the color capsules to be useful for human health in many aspects such as the immune system, heart and eye health.

[0030] In the color capsules of the invention, said anthocyanin extract is present in emulsified form in a primary emulsion that is emulsified in a secondary emulsion. In other words, the color capsules of the invention contain an emulsion-in-emulsion (E / E), also known as a biphasic emulsion. Given that two different emulsion systems are used in the color capsules of the invention, it can be said that the capsules have a hybrid structure.

[0031] In a preferred embodiment of the invention, the primary emulsion comprises an oil phase and a water phase containing the anthocyanin extract emulsified in the said oil phase. Accordingly, the secondary emulsion comprises a biopolymer solution as well as the primary emulsion emulsified in said biopolymer solution. In the preferred embodiment of the invention, the biopolymer solution has the ability to gel under appropriate conditions (interaction with salt and pH=3). According to this embodiment, the color capsules of the invention can also be defined as emulgel capsules. According to an embodiment, the biopolymer solution comprises kappa-carrageenan and sodium alginate.

[0032] The invention also describes the production of the color capsules suitable for use in food products. The method of the invention comprises the following main steps: a. Obtaining an anthocyanin extract from plant raw materials b. Emulsifying the anthocyanin extract in a primary emulsion c. Emulsifying the primary emulsion in a biopolymer-based secondary emulsion in order to obtain a biphasic emulsion d. Forming biphasic emulsion-based gel-form (emulgel) capsules by spraying the biphasic emulsion into a salt bath using an electrospraying technique

[0033] According to an embodiment, said step (a) comprises the following sub-steps: a-i. Preparing a mixture by adding dried purple basil leaves into an alcohol-based solvent a-ii. Subjecting the mixture prepared in step (a-i) to extraction in an ultrasonic bath a-iii. Filtering the extract obtained in step (a-ii) and centrifuging the filtrate a-iv. Removing alcohol from the extract separated at the end of step (a-iii) a-v. Lyophilizing the aqueous extract from which the alcohol was removed in step (a- iv) in order to convert it into powder

[0034] In the preferred embodiment of the invention, said alcohol-based solvent in step (a-i) is an aqueous methanol solution. The alcohol-based solvent is preferably adjusted to pH=3 with acetic acid. According to an embodiment of the invention, a methanokwater ratio in the aqueous methanol solution is 4: 1 by volume.

[0035] In the preferred embodiment of the invention, the ultrasonic wave power in the said ultrasonic bath in step (a-ii) is in the range of 150-200W and the ultrasonic wave frequency is in the range of 30-50 kHz. The extraction process in an ultrasonic bath is mainly based on the fact that sound waves generate microscopic bubbles in the liquid medium, these bubbles burst and break up the particles in the solvent, thereby releasing the content to be extracted from the particles. The efficiency of the extraction process in an ultrasonic bath environment is directly dependent on the wave power and wave frequency parameters. In this respect, wave power is the amount of energy that ultrasonic waves impart to the liquid. A higher wave power results in the formation of more bubbles and more violent explosions. This ensures that the raw material breaks down faster and the substances to be extracted are released in an easier manner. On the other hand, if a higher wave power than it should be is applied, this may cause damage to the raw material and destruction of the substances to be extracted. Wave frequency refers to the vibration rate of the ultrasonic waves. A high wave frequency results in the formation of smaller bubbles and faster explosion. This increases the amount of particle degradation in the solvent, leading the way for the substances to be extracted to be released in smaller particles. However, when the wave frequency is applied at higher values than it should be, it can make it difficult for bubbles to form and reduce the efficiency of the extraction process. According to an embodiment, the ultrasonic wave power in the ultrasonic bath is set to 180W and the ultrasonic wave frequency is set to 40 kHz.

[0036] The temperature of the ultrasonic bath and the duration of the extraction process are, among others, important factors that play an important role in the extraction process with an ultrasonic bath. Temperature has a significant effect on the rate and efficiency of the extraction process. While high temperatures cause liquid molecules to move faster and facilitate the formation of bubbles, if the temperatures reach a higher level than the necessary, the pigments and antioxidant content that are desired to be extracted may be damaged. Similarly, an extraction process that takes longer than the necessary may cause decomposition of anthocyanins and / or the loss of antioxidant properties. According to a preferred embodiment, said extraction process in step (a-ii) is carried out at 40-50°C for 20-40 minutes, more preferably at 45°C for 30 minutes. The value ranges specified in the invention are determined by taking into account the coordinated relationship between the temperature and time, and the structure of the plant particles in the solvent as well as the structure of the anthocyanins desired to be extracted from the raw material.

[0037] In the preferred embodiment of the invention, said filtering process in step (a-iii) is performed using a filter paper. Said filter paper preferably has a pore size in the range of 10-20 pm. Again, in this step, said centrifugation is carried out at an acceleration of 2000- 3000xg and at a temperature of 2-10°C for 10-20 minutes. Here, the value given in the unit "xg" indicates how many times greater force than the gravity is applied to the filtrate. The acceleration of gravity is lg. Accordingly, 2000-3000xg means that a force of 2000 to 3000 times greater than the gravity is applied. The acceleration value range specified herein is selected based on the size of the particles centrifuged, as well as the density and viscosity of the filtrate. The temperature range is selected taking into account the freezing point of the solvent. The aim is to select a temperature just above the freezing point of the solvent in order to slow down any chemical reactions that may occur in the solution centrifuged and facilitate the settlement of the particles. The time interval is the time required for all particles to settle. In the preferred embodiment of the invention, the centrifugation process in step (a-iii) is performed at an acceleration of 2576xg and at a temperature of 4°C for 15 minutes.

[0038] In an embodiment of the invention, the removal of alcohol in step (a-iv) is performed in a rotary vacuum evaporator set to a temperature range of 30-50°C. Step (a-iv) is preferably performed under a vacuum of 60-100 mbar. The evaporation process is used to separate a low boiling point component, such as alcohol, from a compound with a relatively higher boiling point. Therefore, when determining the temperature range specified in step (a-iv), the boiling point of the solvent selected in step (a-i) is taken into account. Accordingly, an evaporation temperature in the range of 30-50°C is determined taking into account that the boiling point of the solvent used will vary in the range of 60-80°C. The reason why the evaporation temperature determined herein is selected to be lower than the boiling temperature of the solvent is to ensure that the solvent is removed without degradation, also saving energy. In the preferred embodiment of the invention, the temperature of the rotary vacuum evaporator is set at 40°C.

[0039] According to an embodiment of the invention, said lyophilization in step (a-v) is performed at a temperature range of -55°C to -80°C, at a pressure of 1 hPa, for 48-72 hours depending on the water content of the material. The powdered product obtained from this step comprises anthocyanins obtained from purple basil leaves.

[0040] According to an embodiment, step (b) of the main steps in the method of the invention comprises the following sub-steps: b-i. Preparing an internal water phase (Wl) containing the anthocyanin extract in powder form b-ii. Combining the internal water phase (Wl) prepared in step (b-i) with an external oil phase (O) and a lipophilic emulsifier b-iii. Mixing the composition prepared in step (b-ii)

[0041] In an embodiment of the invention, said internal water phase in step (b-i) comprises anthocyanin extract in a proportion ranging from 0.1% to 2% (w / v). In the preferred embodiment of the invention, this ratio is 1% (w / v). In the same step, the internal water phase (Wl) is adjusted to pH=3-3.5 with 0.1 M acetate buffer. In an embodiment of the invention, said external oil phase (O) in step (b-ii) comprises at least one of the sunflower oil, corn oil, soybean oil, and canola oil. In the preferred embodiment of the invention, the external oil phase (O) consists of sunflower oil. In an embodiment of the invention, polyglycerol polyricinoleate or lecithin is used as an emulsifier in step (b-ii) to form the primary emulsion of the internal water phase (Wl) and the external oil phase (O). In an optional embodiment of the invention, the ratios of the internal water phase (Wl), the external oil phase (O) and the emulsifier in the said composition in step (b-ii) are respectively 40:57:3 by weight. In step (b-iii), a high-speed disperser (e.g. ultra-turrax, HG15D, Daihan) is preferably used for mixing. In an embodiment of the invention, said mixing in step (b-iii) is carried at a speed of 10000-15000 rpm for 10-20 minutes, more preferably at 13750 rpm for 15 minutes. The mixing values herein ensure that the primary emulsion is disintegrated into small droplets and dispersed homogeneously. The mixing speed and time values recommended within the scope of the invention increase a surface area between the internal water phase (Wl) and the external oil phase (O), thereby allowing a higher amount of emulsifier to adsorb onto the droplet surface. This prevents the separation of the water phase and the oil phase and increases the stability of the emulsion.

[0042] According to an embodiment, step (c) of the main steps in the method of the invention comprises the following sub-steps: c-i. Preparing a biopolymer solution c-ii. Combining the primary emulsion with a hydrophilic emulsifier and a biopolymer solution c-iii. Mixing the composition prepared in step (c-ii)

[0043] In the preferred embodiment of the invention, said biopolymer solution in step (c-i) forms the external water phase (W2) in the secondary emulsion. Said biopolymer solution, also known as the external water phase (W2), comprises sodium alginate (SA) and kappa- carrageenan (K-CG). Here, the total ratio of SA and K-CG in the biopolymer solution is preferably 2% (w / v). In the preferred embodiment of the invention, said biopolymer solution comprises sodium alginate (SA) and kappa-carrageenan (K-CG) dissolved in 0.1 M acetate buffer at pH=3-3.5. According to an embodiment of the invention, the ratio of SA: K-CG in the acetate buffer is in the range of 1:0.05 to 1:0.5 by weight.

[0044] Accordingly, in step (c-i), first of all the acetate buffer is heated to a temperature in the range of 70-90°C, preferably 80°C, and K-CG is added thereto at the determined rate and mixed. In an embodiment of the invention, said mixing process is carried out in a magnetic stirrer at a rate of 500-1000 rpm for 2-3 hours. The mixing preferably takes 2 hours at 600 rpm. Subsequently, the mixture is cooled to a temperature between 40°C and 55°C, SA is added thereto, and the mixing process is continued at the same mixing speed, preferably for another 2-3 hours.

[0045] The biopolymer solution prepared in step (c-i), namely the external water phase (W2), is combined with the primary emulsion (Wl-O) consisting of the internal water phase (Wl) and the external oil phase (O) in step (c-ii) in the presence of a hydrophilic emulsifier. In an optional embodiment of the invention, said emulsifier in step (c-ii) comprises polysorbate 80 (Tween 80). In an optional embodiment of the invention, the ratio of the primary emulsion (Wl-O) in the said composition in step (c-ii) to the biopolymer solution (W2) also containing the hydrophilic emulsifier is 30:70 by weight. The ratio of the said hydrophilic emulsifier in the biopolymer solution (W2) is in the range of 0.1-1% (w / v).

[0046] The composition formed in step (c-ii) is mixed in step (c-iii) and thus a biphasic and gelform emulsion (W1-0-W2) is formed. A high-speed disperser (e.g. ultra-turrax, HG15D, Daihan) is preferably used for mixing. In an embodiment of the invention, said mixing in step (c-iii) is performed at a rate of 10000-15000 rpm for 3-10 minutes, more preferably at 11000 rpm for 4 minutes. The recommended value ranges for the mixing speed and time gently surround the small droplets in the primary phase, ensuring the formation of a stable secondary emulsion. With the lower speed and time values selected for step (c-iii) as compared to step (b-iii), excessive mixing of the composition is avoided, thus preventing the droplets in the primary phase from agglomerating and destabilizing the emulsion.

[0047] According to an embodiment, step (d) of the main steps in the method of the invention comprises the following sub-steps: d-i. Preparing a salt bath d-ii. Introducing a biphasic emulsion into an electrospinning unit d-iii. Adjusting a distance between the salt bath and a syringe tip from which the spraying is to be performed d-iv. Spraying the biphasic emulsion into the salt bath in order to form biphasic gel-form emulsion capsules in the salt bath d-v. Filtering the gel-form capsules obtained in step (d-iv), after being kept at room conditions, and washing them with distilled water d-vi. Drying the capsules washed in step (d-v)

[0048] In the preferred embodiment of the invention, said salt bath in step (d-i) comprises CaCI2 and KCI salts. The salt content in the salt bath is between 5-20% (w / v). The ratio of CaCI2 and KCI salts in the bath may range from 1: 10 to 10: 1 by weight. Said salts are selected in accordance with the content of the biopolymer solution. Sodium alginate interacts strongly with Ca2+ions. Ca2+ions form cross-links with the carboxylate groups in the alginate chains. This cross-linking creates a gel-like structure and increases the stability of the emulsion. Kappa-carrageenan interacts with K+ ions and promotes gel formation. The distance from which the biphasic emulsion is sprayed into the salt bath is important in terms of the size and shape of the final capsules formed. When the spraying distance is relatively short, the droplets reach the salt bath faster and the cross-linking takes place faster. This can result in larger and irregular capsules, because the droplets are forced to gel in a shorter period of time. If the said distance is kept relatively longer, this extends the time it takes for the droplets to reach the salt bath. This allows the droplets to become smaller and more homogeneous, paving the way for obtaining uniform-sized capsules. However, long distances may also cause stability problems. Therefore, the distance should be kept at an ideal value. According to an embodiment of the invention, said distance in step (d-iii) is in the range of 5-10 cm. In the preferred embodiment, said distance in step (d-iii) is set to 10 cm. It is observed that it is possible to obtain homogeneous, propershaped and stable capsules with the distance values as determined in the invention.

[0049] The parameters used in the electrospraying process, such as voltage, current, feeding rate and the diameter of the syringe tip are interrelated, each of which affects the formation of droplets, size and emulsion properties. The voltage determines the magnitude of the electrostatic forces during the electrospraying process and causes an increase in the charges on the surface of the liquid, thereby breaking the surface tension. This allows the atomization of the liquid, i.e., to be sprayed in the form of small droplets. An increase in the voltage may assist in generation of smaller droplets and obtaining a more uniform spray pattern, while voltages that are too high can cause uneven spraying and droplet coalescence. On the other hand, the current value is indicative of the electrical conductivity of the liquid during spraying. Generally, the current level increases with the voltage. Maintaining a proper voltage-current balance is important for stable spraying. The feeding rate affects the droplet size and the spraying pattern. The inner diameter of the syringe tip is linearly related to the spraying velocity and the droplet size of the liquid. The tips having relatively small diameters allow for the formation of finer droplets, which helps to achieve more uniform and smaller particles. The feeding rate and the diameter of the syringe tip should also be adjusted coordinately. For example, a relatively high feeding rate will generally produce larger droplets, but a syringe tip with a small diameter can help to tolerate this effect. However, higher voltages allow smaller droplets to be formed at lower feeding rates. If the feeding rate is increased, this may also require increasing the voltage values. In an embodiment of the invention, said spraying in step (d-iv) is performed at a voltage of 6-12 kV and current values of 1-1.5 pA, taking into account all the above factors. According to an embodiment of the invention, in step (d-iv), the feeding rate is set to 0.5- 1.5 mL / h, preferably 1.2 miyh, and according to this embodiment, a syringe tip with an inner diameter value in the range of 0.1-1 mm is used. In the preferred embodiment of the invention, a 21G syringe tip is used. The term "21G syringe tip" refers to the diameter of syringe tips used in electrospraying devices. Here, the letter "G" stands for Gauge. 21G syringe tips have an inner diameter of approximately 0.51 mm and an outer diameter of approximately 0.82 mm. In step (d-iv), the droplets of the biphasic emulsion sprayed into the salt bath form a gel therein and form capsule structures (emulgel capsules). According to this embodiment, (d-iv) the particle diameters of the wet (uncured) capsules obtained from the droplets sprayed from a distance of 5-10 cm with a 21G syringe tip vary in the range of 700-1100 pm. For non-spherical capsules (e.g. elliptical or ovoid), this value can be considered as a length value in the range of 700-1100 pm. According to a preferred embodiment, a 21G syringe tip is used and the distance of the syringe tip to the salt bath is set at 10 cm. According to this embodiment, the average particle diameter of the wet capsules obtained in step (d-iv) is in the range of 1000-1100 pm. For non-spherical capsules (e.g. elliptical or ovoid), this value can be considered as a length value in the range of 1000- 1100 pm.

[0050] According to an embodiment of the invention, said waiting period in step (d-v) is in the range of 10-20 minutes, preferably 15 minutes. Thereafter, the washing process is preferably applied more than once. Then, in step (d-vi), the emulgel capsules are placed in a lyophilizer for drying and subjected to the drying process at a temperature of -55°C to - 80°C (preferably -55°C) and a pressure of lhPa for 12-24 hours. According to an embodiment of the invention, at the end of the drying process, the average particle sizes of the emulgel capsules become smaller as compared to the wet capsules and reach the diameter values in the range of 100-500 pm. For non-spherical capsules (e.g. elliptical or ovoid), this value can be considered as a length value in the range of 100-500 pm.

[0051] The anthocyanin-containing color capsules obtained by the method of the invention are suitable for use as colorants and antioxidants in food products and / or cosmetic products and / or pharmaceutical products. In this way, the health risks caused by synthetic colorants are eliminated, while at the same time the nutritional value of the colored products is increased. More importantly, in the emulgel capsules of the invention, especially bioaccessibility, stability and shelf life are extended compared to the encapsulated anthocyanin systems (e.g. hydrogel capsules) in the art.

Claims

CLAIMS1. A color capsule for use in food products, comprising a primary emulsion emulsified in a biopolymer-based, gel-form secondary emulsion, and an anthocyanin extract emulsified in the primary emulsion.

2. The color capsule according to claim 1, wherein the anthocyanin extract is made from purple basil leaves.

3. The color capsule according to claim 1 or 2, wherein the primary emulsion comprises an oil phase and a water phase containing the anthocyanin extract emulsified in the oil phase.

4. The color capsule according to claim 3, wherein the secondary emulsion comprises a biopolymer solution and the primary emulsion emulsified in the biopolymer solution.

5. The color capsule according to claim 4, wherein the biopolymer solution comprises kappa-carrageenan and sodium alginate.

6. A method for the production of color capsules for use in food products, comprising the following main steps: a. Obtaining an anthocyanin extract from plant raw materials b. Emulsifying the anthocyanin extract in a primary emulsion c. Emulsifying the primary emulsion in a biopolymer-based secondary emulsion to obtain a biphasic emulsion d. Forming biphasic emulsion-based gel-form capsules by spraying the biphasic emulsion into a salt bath using electrospraying technique7. The method according to claim 6, wherein step (a) comprises the following sub-steps: a-i. Preparing a mixture by adding dried purple basil leaves into an alcohol-based solvent a-ii. Subjecting the mixture prepared in step (a-i) to extraction in an ultrasonic bath a-iii. Filtering the extract obtained in step (a-ii) and centrifuging the filtrate a-iv. Removing alcohol from the extract separated at the end of step (a-iii) a-v. Dissolving the extract from which the alcohol was removed in step (a-iv) in water and lyophilizing extract to convert the extract into powder8. The method according to claim 7, wherein the alcohol-based solvent in step (a-i) is an aqueous methanol solution adjusted to pH=3 with acetic acid.

9. The method according to claim 8, wherein the ratio of methanol: water in the methanol solution is 4: 1 by volume.

10. The method according to any one of claims 7 to 9, wherein the ultrasonic wave power in the ultrasonic bath in step (a-ii) is in the range of 150-200W and the ultrasonic wave frequency is in the range of 30-50 kHz.

11. The method according to claim 10, wherein said extraction process in step (a-ii) is carried out at a temperature of 40-50°C for 20-40 minutes.

12. The method according to any one of claims 7 to 11, wherein said filtering process in step (a-iii) is performed using a filter paper having a pore size of 10-20 pm.

13. The method according to any one of claims 7 to 12, wherein said centrifugation in step (a-iii) is carried out at an acceleration of 2000-3000xg, and at a temperature of 2-10°C for 10-20 minutes.

14. The method according to any one of claims 7 to 13, wherein the removal of alcohol in step (a-iv) is performed in a rotary vacuum evaporator set to a temperature in the range of 30-50°C, and under a vacuum of 60-100mbar.

15. The method according to any one of claims 7 to 14, wherein said lyophilization process in step (a-v) is performed at a temperature of -55°C to -80°C and a pressure of 1 hPa for 48-72 hours.

16. The method according to any one of claims 6 to 15, wherein step (b) comprises the following sub-steps: b-i. Preparing an internal water phase containing the anthocyanin extract in powder form b-ii. Combining the internal water phase prepared in step (b-i) with an external oil phase and a lipophilic emulsifier b-iii. Mixing the composition prepared in step (b-ii)17. The method according to claim 16, wherein the internal water phase in step (b-i) comprises 0.1-2% (w / v) of the anthocyanin extract.

18. The method according to claim 16 or 17, wherein the internal water phase in step (b- i) is adjusted to pH=3-3.5 with 0.1 M acetate buffer.

19. The method according to any one of claims 16 to 18, wherein the external oil phase in step (b-ii) comprises at least one of the sunflower oil, corn oil, soybean oil, and canola oil.

20. The method according to any one of claims 16 to 19, wherein the lipophilic emulsifier in step (b-ii) comprises polyglycerol polyricinoleate or lecithin.

21. The method according to any one of claims 16 to 20, wherein the ratio of the internal water phase, the external oil phase and the emulsifier in the said composition in step (b-ii) is 40:57:3 by weight, respectively.

22. The method according to any one of claims 16 to 21, wherein said mixing in step (b- iii) is performed at a speed of 10000-15000 rpm for 10-20 minutes.

23. The method according to any one of claims 6 to 22, wherein step (c) comprises the following sub-steps: c-i. Preparing a biopolymer solution c-ii. Combining the primary emulsion with a hydrophilic emulsifier and a biopolymer solution c-iii. Mixing the composition prepared in step (c-ii)24. The method according to claim 23, wherein the biopolymer solution in step (c-i) comprises sodium alginate and kappa-carrageenan.

25. The method according to claim 24, wherein the total ratio of sodium alginate and kappa-carrageenan in the biopolymer solution is 2% (w / v).

26. The method according to claim 25, wherein the ratio of sodium alginate to kappa- carrageenan in the biopolymer solution is between 1:0.05 and 1:0.5 by weight, respectively.

27. The method according to any one of claims 23 to 26, wherein, in step (c-i), sodium alginate and kappa-carrageenan are dissolved in 0.1 M acetate buffer at pH=3-3.5 and 70-90°C.

28. The method according to any one of claims 23 to 27, wherein the emulsifier in step (c- ii) is polysorbate 80.

29. The method according to any one of claims 23 to 28, wherein, in step (c-ii), the ratio of the primary emulsion to the biopolymer solution also containing the hydrophilic emulsifier is 30:70 by weight.

30. The method according to claim 29, wherein the ratio of the hydrophilic emulsifier in the biopolymer solution is in the range of 0.1-1% by weight (w / v).

31. The method according to any one of claims 23 to 30, wherein said mixing in step (c- iii) is performed at a speed of 10000-15000 rpm for 3-10 minutes.

32. The method according to any one of claims 6 to 31, wherein step (d) comprises the following sub-steps: d-i. Preparing a salt bath d-ii. Introducing the biphasic emulsion into an electrospinning unit d-iii. Adjusting a distance between the salt bath and a syringe tip from which the spraying is to be performed d-iv. Spraying the biphasic emulsion into the salt bath to form biphasic gel-form emulsion capsules in the salt bath d-v. Filtering the capsules obtained in step (d-iv), after being kept at room conditions, and washing them with distilled water d-vi. Drying the capsules washed in step (d-v)33. The method according to claim 32, wherein the salt bath in step (d-i) comprises CaCI2 and KCI salts.

34. The method according to claim 33, wherein the total ratio of CaCI2 and KCI salts in the bath is between 5-20% (w / v).

35. The method according to claim 33 or 34, wherein the ratio of CaCI2 salts to KCI salts in the bath is between 1: 10 and 10: 1 by weight.

36. The method according to any one of claims 32 to 35, wherein the distance in step (d- iii) is between 5-10 cm.

37. The method according to any one of claims 32 to 36, wherein said spraying process in step (d-iv) is performed at a voltage of 6-12 kV and a current value of 1-1.5 pA.

38. The method according to any one of claims 32 to 37, wherein said spraying process in step (d-iv) is performed with a syringe tip with an inner diameter of 0.1-1 mm and at a feeding rate of 0.5-1.5 mL / h.

39. The method according to any one of claims 32 to 38, wherein said waiting period in step (d-v) is between 10-20 minutes.

40. The method according to any one of claims 32 to 39, wherein said drying process in step (d-vi) is performed in a lyophilizer at a temperature of -55°C to -80°C and a pressure of 1 hPa for 12-24 hours.

41. Use of the color capsules produced by a method according to any one of claims 6 to 40 as colorants and antioxidants in food products and / or cosmetic products and / or pharmaceutical products.

Citation Information

Patent Citations

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