Dry emulsion with solid nanocore containing high amount of ceramide and method for producing same

Abstract

The present invention relates to a dry emulsion comprising a solid nanocore containing a high amount of ceramide and a method for producing same and, more specifically, to a dry emulsion comprising a uniform solid nanocore and a method for producing same, in which, in a core formation step through a temperature change from high to low temperature by using a spray drying method, supersaturation is induced, thereby improving a ceramide loading rate.

Description

Dry emulsion containing solid nano cores containing high ceramide content and method for producing the same

[0001] The present invention relates to a dry emulsion comprising a solid nano core containing a high content of ceramide and a method for producing the same, and more particularly, to a dry emulsion comprising a uniform solid nano core in which the ceramide loading rate is improved by inducing supersaturation in the core formation step through a temperature change from high to low temperature using a spray drying method, and a method for producing the same.

[0002]

[0003] Ceramide is an essential component that forms the structure and function of the stratum corneum between the keratinocytes that make up the stratum corneum of the skin. It protects the skin from external harmful substances, prevents the leakage of important substances from the body, suppresses inflammation, and strengthens the skin barrier function to prevent moisture evaporation.

[0004] The ceramide content of the epidermis decreases with age, which reduces the epidermis' ability to retain moisture and its barrier function, leading to wrinkles and rough skin. However, it is known that supplementing ceramides can help maintain skin homeostasis and solve the above problems.

[0005] However, ceramide is a poorly soluble substance with a complex structure, manufactured through an acylation reaction between fatty acids and precursor sphingoid bases. When used in cosmetic formulations, it has the problem of low formulation stability and gelation.

[0006] Accordingly, various formulation studies are being conducted to stabilize ceramides within the formulation, but the current methods have limitations such as low ceramide content, complex manufacturing process, and poor stability.

[0007] Due to the above problems, there is a need for the development of a ceramide-containing emulsion that has a high ceramide content and simultaneously exhibits high stability.

[0008]

[0009] The purpose of the present invention is to provide a dry emulsion containing a solid nano core that has a high ceramide content and exhibits high stability, and a method for producing the same, in order to solve the above-mentioned problems.

[0010] The technical problems to be solved by the present invention are not limited to the technical problems mentioned above, and other technical problems not mentioned can be clearly understood by a person having ordinary skill in the art from the description of the present invention.

[0011]

[0012] In order to achieve the above object, the present invention provides a dry emulsion comprising a solid nanocore containing a high content of ceramide, which comprises a solid nanocore containing ceramide and oleic acid; and wall materials containing gum arabic and maltodextrin, and which is in a powdered form through spray drying.

[0013] In the present invention, the solid nano core is characterized by being solidified by dissolving ceramide in oleic acid and then adding polysorbate.

[0014] In the present invention, the oleic acid is characterized in that it is heated at a temperature of 65 to 95°C.

[0015] In the present invention, the ceramide is characterized in that it is included in an amount of 15 to 23 parts by weight based on 100 parts by weight of the dry emulsion.

[0016] In the present invention, the polysorbate is characterized in that it is added in an amount of 1 to 1.5 parts by weight relative to 1 part by weight of the oleic acid.

[0017] In the present invention, the solid nano core is characterized by having a size of 100 to 300 nm.

[0018] In the present invention, the wall is characterized by mixing the gum arabic and the maltodextrin in a weight ratio of (4 to 2): 1.

[0019] In the present invention, the dry emulsion is characterized by having a particle size of 2 to 12 μm.

[0020] In the present invention, the dry emulsion is characterized in that the average particle size is 4 to 8 ㎛.

[0021] The present invention provides a method for producing a dry emulsion including a solid nanocore having a high ceramide content, the method comprising the steps of: heating oleic acid; dissolving ceramide in the heated, high-temperature oleic acid; adding polysorbate to the oleic acid containing the dissolved ceramide to form nanocores; cooling the nanocores to solidify them; mixing gum arabic and maltodextrin; adding the mixed gum arabic and maltodextrin onto the solidified nanocores to form walls; and spray-drying the solid nanocores having the walls formed to produce a powdered dry emulsion.

[0022] In the present invention, the step of heating the oleic acid is characterized by heating it at a temperature of 65 to 95°C.

[0023] In the present invention, the step of dissolving ceramide is characterized by dissolving ceramide at a concentration of 350 to 550 mg / mL.

[0024] In the present invention, the step of dissolving the ceramide is characterized by dissolving 15 to 23 parts by weight based on 100 parts by weight of the dry emulsion.

[0025] In the present invention, the step of forming the nano core is characterized by including the steps of: adding oleic acid containing the ceramide and the polysorbate to a solvent heated to a temperature of 65 to 95° C.; stirring the mixed solution; and homogenizing the stirred mixed solution by ultrasonic treatment.

[0026] In the present invention, the step of adding the oleic acid containing the ceramide and the polysorbate is characterized in that the oleic acid and the polysorbate are added in a weight ratio of 1: (1 to 1.5).

[0027] In the present invention, the step of cooling and solidifying the nano core is characterized by solidifying by cooling and stabilizing at 2 to 6°C.

[0028] In the present invention, the step of mixing the gum arabic and the maltodextrin is characterized in that the gum arabic and the maltodextrin are mixed in a weight ratio of (4 to 2): 1.

[0029] In the present invention, the step of forming the wall is characterized by adding 10 to 20 parts by weight of the mixture of gum arabic and maltodextrin relative to 100 parts by weight of the solidified nanocore.

[0030] In the present invention, the step of preparing a powdered dry emulsion by spray drying is performed at 160 to 200°C and 0.3 to 0.6 m 2 It is characterized by spray drying by atomizing at a blowing speed of / min and a pressure of (13 to 15) × 10 kPa.

[0031]

[0032] By means of solving the above problem, the present invention can provide a dry emulsion including a solid nano core that contains a high amount of ceramide and exhibits high stability, and a method for producing the same.

[0033] In addition, the present invention can provide a dry emulsion including a solid nano core containing a very high amount of ceramide, at least 10% of the total emulsion weight, and a method for producing the same.

[0034] In addition, the present invention can provide a dry emulsion including a solid nanocore exhibiting excellent physical stability under various temperature conditions and a method for producing the same.

[0035] In addition, the present invention can provide a dry emulsion including a solid nano core that can be manufactured in a powder form through spray drying, and a method for manufacturing the same.

[0036] The effects of the present invention are not limited to the effects mentioned above, and other effects not mentioned will be clearly understood by those skilled in the art from the description of the claims.

[0037]

[0038] Figure 1 is a drawing showing a method for producing a solid dry emulsion containing a high amount of ceramide according to the present invention.

[0039] FIG. 2 is a drawing showing a dry emulsion containing a solid nano core containing a high amount of ceramide according to the present invention.

[0040] FIG. 3 is a drawing showing the results of particle size analysis of particles redispersed in Example 1-1, Example 2-1, and Example 2-1 according to the present invention.

[0041] FIG. 4 is a drawing showing the results of particle size analysis of particles redispersed in Examples 1-2, 2-2, and 2-2 according to the present invention.

[0042] FIG. 5 is a drawing showing the results of particle size analysis of redispersed particles of Examples 1-3, 2-3, and 2-3 according to the present invention.

[0043] FIG. 6 is a drawing showing the results of particle size analysis of particles redispersed in Examples 1-4, 2-4, and 2-4 according to the present invention.

[0044] FIG. 7 is a drawing showing the results of particle size analysis of particles redispersed in Examples 1-5, 2-5, and 2-5 according to the present invention.

[0045] Figure 8 is a drawing showing the results of SEM analysis of a dry emulsion containing a solid nano core of Example 2-1 according to the present invention.

[0046] Figure 9 is a drawing showing the results of SEM analysis of a dry emulsion containing a solid nano core of Example 2-2 according to the present invention.

[0047] Figure 10 is a drawing showing the results of SEM analysis of a dry emulsion containing solid nanocores of Example 2-3 according to the present invention.

[0048] Figure 11 is a drawing showing the results of SEM analysis of a dry emulsion containing solid nanocores of Example 2-4 according to the present invention.

[0049] Figure 12 is a drawing showing the results of SEM analysis of a dry emulsion containing solid nanocores of Example 2-5 according to the present invention.

[0050] Figure 13 is a drawing showing the results of FT-IR analysis of gum arabic, maltodextrin, polysorbate 80 (Tween 80), oleic acid, and ceramide according to the present invention.

[0051] FIG. 14 is a drawing showing the results of FT-IR analysis of dry emulsions containing solid nanocores of Examples 2-1 to 2-5 according to the present invention.

[0052] FIG. 15 is a diagram showing the results of DSC analysis of a dry emulsion containing ceramide according to the present invention and solid nanocores of Examples 2-1 to 2-5.

[0053] FIG. 16 is a drawing showing the results of XRD analysis of a dry emulsion containing ceramide according to the present invention and solid nanocores of Examples 2-1 to 2-5.

[0054] Figure 17 is a drawing showing the results of evaluating the storage stability at a temperature of 4°C of Examples 2-1 to 2-5 according to the present invention.

[0055] Figure 18 is a drawing showing the results of evaluating the storage stability at a temperature of 25°C of Examples 2-1 to 2-5 according to the present invention.

[0056] Figure 19 is a drawing showing the results of evaluating the storage stability at a temperature of 40°C of Examples 2-1 to 2-5 according to the present invention.

[0057]

[0058] The terms used in this specification have been selected from widely used, current terms, taking into account the functions of the present invention. However, these terms may vary depending on the intentions of those skilled in the art, precedents, the emergence of new technologies, etc. Furthermore, in certain cases, terms may be arbitrarily selected by the applicant, in which case their meanings will be described in detail in the relevant description of the invention. Therefore, the terms used in this invention should not be defined simply as names, but rather based on their inherent meanings and the overall content of the present invention.

[0059] Unless otherwise defined, all terms used herein, including technical or scientific terms, have the same meaning as commonly understood by one of ordinary skill in the art to which this invention pertains. Terms defined in commonly used dictionaries should be interpreted as having a meaning consistent with their meaning in the context of the relevant technology, and shall not be interpreted in an idealized or overly formal sense unless explicitly defined herein.

[0060] Numerical ranges are inclusive of the values ​​defined in the ranges above. Any maximum numerical limitation given throughout this specification includes any lower numerical limitation, as if that lower numerical limitation were explicitly stated. Any minimum numerical limitation given throughout this specification includes any higher numerical limitation, as if that higher numerical limitation were explicitly stated. Any numerical limitation given throughout this specification will include any better numerical range within the broader numerical range, as if that narrower numerical limitation were explicitly stated.

[0061]

[0062] Dry emulsion containing solid nano cores containing high ceramide content

[0063] The present invention relates to a dry emulsion comprising a solid nano core containing a high content of ceramide.

[0064] The present invention relates to a dry emulsion comprising a solid nanocore containing a high content of ceramide, which comprises a solid nanocore containing ceramide and oleic acid; and wall materials containing gum arabic and maltodextrin, and which is in powdered form through spray drying.

[0065] The dry emulsion containing the solid nanocores containing a high content of ceramide may be one in which the ceramide is completely encapsulated in the solid nanocores inside the wall, so that no ceramide exists on the surface. In addition, the dry emulsion may exhibit a completely spherical and amorphous shape. The dry emulsion powdered through the spray drying may be one that achieves high stability through powderization.

[0066] In the present invention, the solid nanocore may be solidified by dissolving ceramide in oleic acid and then adding polysorbate. The polysorbate may preferably be polysorbate 80.

[0067] In the present invention, the oleic acid may be heated to a temperature of 65 to 95°C, but is not limited thereto. The oleic acid heated to such a high temperature can melt an excess of ceramide that does not dissolve at room temperature.

[0068] In the present invention, the ceramide may be included in an amount of 15 to 23 parts by weight based on 100 parts by weight of the dry emulsion, but is not limited thereto. The dry emulsion may exhibit a ceramide loading rate that is tens to hundreds of times higher than that of conventional emulsions.

[0069] In the present invention, the polysorbate may be added in an amount of 1 to 1.5 parts by weight relative to 1 part by weight of the oleic acid, but is not limited thereto.

[0070] In the present invention, the solid nano core may have a size of 100 to 300 nm, but is not limited thereto.

[0071] In the present invention, the wall may be a mixture of the gum arabic and the maltodextrin in a weight ratio of (4 to 2): 1, but is not limited thereto. The wall formed through the solidification as described above may prevent the ceramide from appearing on the surface of the dry emulsion.

[0072] In the present invention, the dry emulsion may have a particle size of 2 to 12 μm, but is not limited thereto.

[0073] In the present invention, the dry emulsion may have an average particle size of 4 to 8 μm, but is not limited thereto.

[0074]

[0075] Method for producing a dry emulsion containing a solid nano core containing a high content of ceramide

[0076] The present invention relates to a method for producing a dry emulsion comprising a solid nano core containing a high content of ceramide.

[0077] The present invention relates to a method for producing a dry emulsion including solid nanocores having a high ceramide content, the method comprising the steps of: heating oleic acid; dissolving ceramide in the heated, high-temperature oleic acid; adding polysorbate to the oleic acid containing the dissolved ceramide to form nanocores; cooling the nanocores to solidify them; mixing gum arabic and maltodextrin; adding the mixed gum arabic and maltodextrin onto the solidified nanocores to form walls; and spray-drying the solid nanocores with the walls formed to produce a powdered dry emulsion.

[0078] In the present invention, the step of heating the oleic acid may be heating at a temperature of 65 to 95°C, but is not limited thereto. The oleic acid heated at such a high temperature can melt an excess of ceramide that does not dissolve at room temperature.

[0079] In the present invention, the step of dissolving the ceramide may be dissolving the ceramide at a concentration of 350 to 550 mg / mL, but is not limited thereto.

[0080] In the present invention, the step of dissolving the ceramide may be dissolving 15 to 23 parts by weight based on 100 parts by weight of the dry emulsion, but is not limited thereto.

[0081] In the present invention, the step of forming the nano core may include a step of adding oleic acid and the polysorbate containing the ceramide to a solvent heated to a temperature of 65 to 95° C.; a step of stirring the mixed solution; and a step of homogenizing the stirred mixed solution by ultrasonic treatment.

[0082] In the present invention, the step of adding the oleic acid containing the ceramide and the polysorbate may be, but is not limited to, adding the oleic acid and the polysorbate in a weight ratio of 1: (1 to 1.5). The polysorbate may preferably be polysorbate 80.

[0083] In the present invention, the step of cooling and solidifying the nanocore may be, but is not limited to, solidifying by cooling and stabilizing at 2 to 6°C. The manufacturing method may induce the encapsulation of an excess ceramide by melting an excess ceramide at a high temperature and then cooling to a low temperature to induce supersaturation.

[0084] In the present invention, the step of mixing the gum arabic and the maltodextrin may be mixing the gum arabic and the maltodextrin in a weight ratio of (4 to 2): 1, but is not limited thereto.

[0085] In the present invention, the step of forming the wall may be, but is not limited to, adding 10 to 20 parts by weight of the gum arabic and maltodextrin mixture relative to 100 parts by weight of the solidified nanocore. The wall formed through the step may prevent the ceramide from appearing on the surface of the dry emulsion.

[0086] In the present invention, the step of preparing a powdered dry emulsion by spray drying is performed at 160 to 200°C and 0.3 to 0.6 m 2 / min airflow rate and (13 to 15) × 10 kPa pressure may be used for spray drying, but is not limited thereto. The dry emulsion may be powdered through the above-described spray drying to achieve high stability.

[0087]

[0088] Example

[0089] Hereinafter, examples of the present invention will be described in detail, but it is obvious that the present invention is not limited to the following examples.

[0090] The advantages and features of the present invention, and the methods for achieving them, will become clearer with reference to the embodiments described in detail below. However, the present invention is not limited to the embodiments disclosed below and may be implemented in various different forms. The embodiments are provided solely to ensure that the disclosure of the present invention is complete and to fully inform those skilled in the art of the scope of the invention. The present invention is defined solely by the scope of the claims.

[0091]

[0092] <Example 1> Solid nanocore containing high ceramide content

[0093] Oleic acid containing ceramide was prepared by dissolving 450 mg / mL of ceramide in oleic acid heated to 80°C. Thereafter, polysorbate Tween 80 and the oleic acid containing ceramide were added to water heated to 80°C in the ratios shown in [Table 1] below and stirred at 500 rpm for 5 minutes. The stirred mixture was homogenized by ultrasonication (5 sec on, 5 sec off) at 300 W for 1 minute using a probe sonicator (Scientz-IID, Scientz, China), and then the formulation of the mixture was stabilized by ultrasonication for 3 minutes in a cold ultrasonic bath to prepare solid nanocores containing high ceramide, Examples 1-1 to 1-5.

[0094]

[0095]

[0096] <Example 2> Dry emulsion containing solid nanocores containing high ceramide content

[0097] In the solid nanocore manufactured in Example 1, gum arabic and maltodextrin were mixed in a ratio of 3:1 (w / w) as a wall material and mixed in a ratio of 15% (w / v) to the solid nanocore. Afterwards, a spray dryer (EYELA SD-1000, EYELA, Japan) was used at an inlet temperature of 180°C and a blower volume of 0.4-0.5 m 2 / min, and an atomizing pressure of 15×10 kPa were used to obtain dry emulsions containing solid nanocores containing a high content of ceramide, as in Examples 2-1 to 2-5.

[0098]

[0099] <Comparative Example 1> Nano core containing ceramide

[0100] Oleic acid containing ceramide was prepared by dissolving 1 mg / mL of ceramide in oleic acid at room temperature. Thereafter, polysorbate Tween 80 and oleic acid containing ceramide were added to water in the ratios shown in [Table 2] below and stirred at 500 rpm for 5 minutes. The stirred mixture was placed on ice and cooled, and sonicated for 1 minute (5 sec on, 5 sec off) at 300 W using an ultrasonic disrupter (prove sonicator, Scientz-IID, Scientz, China) to homogenize the mixture and prepare ceramide-containing nanocores, Comparative Examples 1-1 to 1-5.

[0101]

[0102]

[0103] <Comparative Example 2> Dry emulsion containing nano cores containing ceramide

[0104] In the nano core manufactured in Comparative Example 1, gum Arabic and maltodextrin were mixed in a ratio of 3:1 (w / w) as a wall material and mixed in a ratio of 15% (w / v) to the nano core. Afterwards, a spray dryer (EYELA SD-1000, EYELA, Japan) was used at an inlet temperature of 180°C and a blower volume of 0.4-0.5 m 2 Comparative Examples 2-1 to 2-5, which are dry emulsions containing nanocores containing ceramide, were obtained by spray drying under the conditions of / min and an atomizing pressure of 15×10 kPa.

[0105]

[0106] <Experimental Example 1> Evaluation of physicochemical properties

[0107] The size, polydispersity index, and zeta potential difference of the solid nanocores manufactured in Examples 1-1 to 1-5 were measured, and the results are shown in [Table 3] below.

[0108] The above measurement was performed using a zetasizer (Nano ZS90, Malvern Instrument, Worcesterishire, UK) after diluting the solid nanocores of Examples 1-1 to 1-5 in water to a concentration of 1% (v / v).

[0109]

[0110] As shown in the above [Table 3], the solid nanocores of Examples 1-1 to 1-5 exhibited particle sizes of approximately 200 nm, and a polydispersity index of less than 0.3, indicating a uniform particle distribution. In addition, all zeta potential differences exhibited negative values.

[0111] Through the above results, it was confirmed that the solid nano core containing a high content of ceramide according to the present invention uniformly exhibits a very small particle size of about 200 nm.

[0112]

[0113] <Experimental Example 2> Storage Stability Evaluation

[0114] The solid nanocores manufactured in Examples 1-1 to 1-5 were stored at 25°C for 4 weeks and the storage stability was evaluated, and the results are shown in [Table 4] below.

[0115] The above evaluation was performed by diluting the solid nanocores of Examples 1-1 to 1-5 in water to a concentration of 1% (v / v) and then measuring them using a zetasizer (Nano ZS90, Malvern Instrument, Worcesterishire, UK).

[0116]

[0117] As shown in the above [Table 4], the solid nanocores of Examples 1-1 to 1-5 maintained their particle size for 4 weeks and exhibited excellent stability.

[0118] Through the above results, it was confirmed that the solid nano core containing a high amount of ceramide according to the present invention exhibits excellent long-term stability.

[0119]

[0120] <Experimental Example 3> Measurement of particle size distribution

[0121] (1) Analysis using a particle size analyzer

[0122] In order to analyze the particle size distribution of the dry emulsion containing the solid nano core containing a high content of ceramide prepared in Examples 2-1 to 2-5, the particle size distribution was measured using a particle size analyzer (990, Anton Paar, Austria), and the results are shown in [Table 5] below.

[0123] The above particle size distribution was measured by a wet method by dispersing at a concentration adjusted to achieve the transmittance level required by the device, and 50% ethanol was used as the dispersion medium. Specifically, the width of the particle size distribution was analyzed using the SPAN value, which was calculated as follows; SPAN = [d(υ, 0.9)-d(υ, 0.1)] / d(υ, 0.5). Here, d(υ, 0.1) means the particle size value that occupies 10% of the entire diameter distribution, d(υ, 0.5) means the median value, and d(υ, 0.9) means the particle size value that occupies 90% of the entire diameter distribution.

[0124]

[0125] As shown in the above [Table 5], the particles of the dry emulsion containing the solid nanocores containing a high content of ceramide of Examples 2-1 to 2-5 exhibited a particle size distribution of about 2 to 12 ㎛, and the average value exhibited a particle size of 4 to 7 ㎛. In addition, the SPAN value exhibited a value of 1.3 to 1.8.

[0126] Through the above results, it was confirmed that the solid nano core containing a high content of ceramide according to the present invention uniformly exhibits a very small particle size.

[0127]

[0128] (2) Particle size analysis after redispersion in water

[0129] The particle size of the dry emulsion containing the solid nano cores containing a high content of ceramide prepared in Examples 2-1 to 2-5 was analyzed using a zetasizer (Nano ZS90, Malvern Instrument, Worcestershire, UK) after redispersing it in water at a concentration of 1% (w / v), and the results are shown in [Table 6] below.

[0130]

[0131] As shown in the above [Table 6], the particle size of the dry emulsion containing the solid nano cores containing a high content of ceramide of Examples 2-1 to 2-5 after redispersion was 370 to 500 nm in size, and the particles were reconstituted due to the heat of spray drying, and the size was found to be 1.9 to 2.4 times larger than before redispersion in the above [Table 5].

[0132] In addition, the redispersion polydispersity index showed a value of 0.08 to 0.13, confirming that it was more uniform than before spray drying. The redispersion zeta potential difference showed a negative value and did not show a large difference from before spray drying.

[0133] Through the above results, it was confirmed that the emulsion manufactured through the spray drying step of the method for manufacturing a dry emulsion including a solid nano core containing a high content of ceramide according to the present invention uniformly exhibits a very small particle size.

[0134]

[0135] (3) Particle size analysis before and after redispersion

[0136] The particle sizes of the solid nanocores manufactured in Examples 1-1 to 1-5 and the dry emulsions manufactured in Examples 2-1 to 2-5 and the particles after redispersion thereof were analyzed, and the results thereof are shown in Figures 3 to 7.

[0137] As shown in FIGS. 3 to 7, the solid nanocores of Examples 1-1 to 1-5 exhibited a narrow distribution of very small particle sizes and a high volume percentage.

[0138] The dry emulsions of Examples 2-1 to 2-5 above exhibited larger particle sizes than the solid nanocores, but smaller volume percentages. After redispersion of the dry emulsions of Examples 2-1 to 2-5, the particle sizes became smaller, while the volume percentages became very high, indicating that the particles were reconstituted due to the heat of spray drying.

[0139] Through the above results, it was confirmed that the solid nano core containing a high content of ceramide according to the present invention uniformly exhibits a very small particle size, and that the emulsion manufactured through the spray drying step according to the manufacturing method of the present invention uniformly exhibits a very small particle size.

[0140]

[0141] <Experimental Example 4> Measurement of ceramide content in formulations

[0142] The ceramide content of the dry emulsions containing the nanocores containing ceramide prepared in Examples 2-1 to 2-5 and Comparative Examples 2-1 to 2-5 was measured using high-performance liquid chromatography (HPLC, Agilent 1100 Series, Agilent Technologies, CA, USA), and the results are shown in [Table 7] below.

[0143] To measure the ceramide content, a mixture of chloroform and water (1:1, v / v) was added to the dry emulsion powder of Examples 2-1 to 2-5 to separate the wall from the internal oil, and the mixture was thoroughly mixed using a vortex mixer. Water was removed from the mixture, leaving only the chloroform, and the mixture was completely dried to obtain a dried product. The dried product was then subjected to a deacylation reaction for analysis.

[0144] The above deacylation reaction was carried out using sphingolipid ceramide N-deacylase (SCDase), an enzyme that hydrolyzes sphingolipids into lysisphingolipids and fatty acids. For the deacylation reaction, the dried product was mixed in an enzyme reaction solution containing 15% fatty acid-free bovine serum albumin, 1% sodium cholate, 25 mM Tris-HCl buffer (pH 7.5), and 150 μU SCDase. Afterwards, the enzyme reaction was promoted by gently mixing for 12 hours in an isothermal shaker (JSSI-100C, JS Research, Republic of Korea) at 37°C.

[0145] After completing the above enzyme reaction, the enzyme reaction solution was added 3 times with ethanol to precipitate the bovine serum albumin used in the enzyme reaction, and then centrifuged to remove it. The supernatant was dried using nitrogen. Next, the dried material was resuspended in methanol and treated with OPA reagent for fluorescence derivatization. At this time, the OPA reagent was composed of o-phthaldialdehyde, Brij® 35, methanol, 2-mercaptoethanol, potassium hydroxide, and boric acid (pH 10.4). The OPA reagent treatment was carried out in a darkroom for 30 minutes, and then quantitative analysis was performed using an Agilent 1100 series HPLC and an ODS Ⅱ column (Supersil 120 ODS Ⅱ, 4.6 × 150 mm, 5 μm, LB Science, Busan, Republic of Korea). In the analysis using the above HPLC-FLD, the mobile phase consisted of methanol / distilled water (92:8, v / v), and the flow rate was maintained at 1 mL / min. The fluorescence detector was set to an excitation wavelength of 340 nm and an emission wavelength of 455 nm.

[0146]

[0147] The above content increase rate is (ceramide content of Examples 2-1 to 2-5) / (ceramide content of Comparative Examples 2-1 to 2-5) x 100 (%).

[0148] As shown in the above [Table 7], the ceramide-containing dry emulsions of Comparative Examples 2-1 to 2-5 exhibited a dry weight of 0.02 to 0.07 g per 100 g of the formulation, and the dry emulsions containing solid nanocores with a high content of ceramide of Examples 2-1 to 2-5 exhibited a dry weight of 16 to 23 g per 100 g of the formulation.

[0149] Specifically, in formulations containing the same ratio of oil and surfactant, it was confirmed that the ceramide content of formulations prepared using the supersaturation method at high temperature in Examples 2-1 to 2-5 increased by 232 to 980 times compared to formulations prepared using the general method at room temperature in Comparative Examples 2-1 to 2-5.

[0150] Through the above results, it was confirmed that the method of manufacturing a solid nano core using a supersaturation method at high temperature according to the method of manufacturing a dry emulsion including a solid nano core containing a high content of ceramide of the present invention can drastically improve the ceramide content in the formulation.

[0151]

[0152] <Experimental Example 5> Appearance Analysis of High-Ceramide-Content Solid Core-Dry Emulsion

[0153] (1) Scanning Electron Microscope (SEM)

[0154] In order to analyze the appearance of the dry emulsion containing the solid nano core containing a high content of ceramide prepared in Examples 2-1 to 2-5, surface images were taken using a field emission scanning electron microscope (FE-SEM, JEOL, JSM-7800F), and the results are shown in Figs. 8 to 12.

[0155] Specifically, before taking the SEM image, the dry emulsion powders of Examples 2-1 to 2-5 were placed on a double-sided adhesive carbon tape and coated with platinum, and images were taken at a magnification of 5,000 times using an electron beam of 5 kV. As shown in FIGS. 8 to 12, the dry emulsions of Examples 2-1 to 2-5 had a smooth surface, and it was found that no oil or ceramide was present on the surface of the dry emulsions.

[0156]

[0157] (2) Fourier transform infrared spectrometer

[0158] In order to confirm whether ceramide exists on the surface of the dry emulsion containing the solid nano core containing a high content of ceramide prepared in Examples 2-1 to 2-5, the dry emulsions of Examples 2-1 to 2-5 and gum arabic, maltodextrin, Tween 80, oleic acid and ceramide included in the dry emulsion were subjected to surface analysis using a Fourier transform infrared spectroscopy (FT-IR, Alpha Ⅱ-Eco, BRUKER, USA), and the results thereof are shown in Figures 13 to 14.

[0159] Specifically, the dry emulsions of Examples 2-1 to 2-5 were placed on an attenuated total reflection (ATR) crystal and measured at 4,000 to 500 cm -1 4 cm in range -1 All analyses were performed at room temperature, and all residue analyses were performed using Brucker OPUS software.

[0160] As shown in Fig. 13, the ceramide has a molecular weight of 2,916.84 cm -1 Asymmetrically elongated C-H2 at 2,849.21 cm -1 C-H2, which is symmetrically elongated at 1,612.15 and 1,556.60 cm, respectively -1 It was confirmed that the oleic acid exhibited characteristic amide I and amide II vibrations at 2,916.84 and 2,849.21 cm -1 C-H2 stretching asymmetric and symmetric motions at 1,707.71 cm -1 Carbonyl stretching vibrations at 1,283.93, 934.43, and 722.3 cm -1 The skeletal vibration was shown in . The above Tween 80 was 2,916.84 and 2,849.21 cm -1 C-H2 stretching asymmetric and symmetric behavior at 1,735.22 cm -1C=O stretching vibration at 1,093.82 cm -1 The COC stretching vibration peak was observed at 1,012-1,075 cm , which corresponds to the CO stretching vibration, for both the maltodextrin and the gum arabic used as wall materials. -1 It showed a peak reaching .

[0161] In addition, as shown in Fig. 14, the dry emulsions of Examples 2-1 to 2-5 had wavelengths of 1,612 and 1,556 cm -1 It was found that the characteristic peaks of ceramide, amide I and amide II vibrations, found in the dry emulsion were not observed. Specifically, it was found that the ceramide was well integrated into the wall of the dry emulsion and was barely present on the surface.

[0162]

[0163] (3) Thermal analysis using differential scanning calorimetry

[0164] In order to confirm the thermal behavior and phase transition of the dry emulsion containing the solid nano core containing a high content of ceramide prepared in Examples 2-1 to 2-5, analysis was performed using a differential scanning calorimeter (DSC-60, Shimadzu, Japan), and the results are shown in Fig. 15.

[0165] Specifically, 6 to 8 mg of ceramide and the dry emulsions of Examples 2-1 to 2-5 were placed in a standard aluminum pan, sealed with a lid, and the aluminum pan was heated from 15 to 30°C using air at a heating rate of 10°C / min.

[0166] As shown in Fig. 15, the ceramide exhibited a melting point of 102.56°C. However, in the dry emulsions of Examples 2-1 to 2-5, no peak indicating the melting point of ceramide appeared. This indicates that there was almost no ceramide present on the particle surface of the dry emulsions of Examples 2-1 to 2-5, and that the ceramide was completely captured by the walls of the dry emulsion. In addition, it can be confirmed that the dry emulsion was in an amorphous state without a peak related to the crystallinity and melting temperature.

[0167]

[0168] (4) X-ray diffraction analysis

[0169] The X-ray diffraction pattern of the dry emulsion containing the solid nano core containing a high content of ceramide prepared in Examples 2-1 to 2-5 was analyzed using X-ray diffraction analysis (XRD, Ultima IV, Rigaku Corp., Japan), and the results are shown in Fig. 16.

[0170] Specifically, measurements were made using Cu-Kα radiation (λ = 1.54 A), and the ceramide and the dry emulsions of Examples 2-1 to 2-5 were placed in an aluminum holder and scanned at 40 kV and 40 mA at a scan rate of 5° / min. Data were collected from 5 to 60° (2θ).

[0171] As shown in Fig. 16, the ceramide exhibited a prominent peak at 6.88° in the XRD pattern, confirming that the ceramide had a high degree of crystallinity.

[0172] However, in the case of the dry emulsions of Examples 2-1 to 2-5, no significant peak was observed, and they were amorphous. Specifically, considering that both gum arabic and maltodextrin, which serve as wall materials, are amorphous, it appeared that the dry emulsions maintained an amorphous state due to the encapsulation of ceramides by gum arabic and maltodextrin.

[0173]

[0174] Through the above results, it was confirmed that the dry emulsion containing the solid nanocore containing a high content of ceramide according to the present invention was completely captured within the wall, and that no ceramide was present on the surface. In addition, it was confirmed that the dry emulsion exhibited a completely spherical shape and was amorphous.

[0175]

[0176] <Experimental Example 6> Storage Stability Evaluation

[0177] The dry emulsions containing solid nanocores containing a high content of ceramide prepared in Examples 2-1 to 2-5 were stored for 7 days under temperature conditions of 4°C, 25°C, and 40°C to evaluate their storage stability, and the results are shown in Figures 17 to 19.

[0178] The above storage stability evaluation was performed by measuring the particle size distribution of the dry emulsion using a particle size analyzer (990, Anton Paar, Austria). All particle size distribution measurements were performed using a wet method by dispersing at a concentration adjusted to achieve the required transmittance level for the device. At this time, 50% ethanol was used as the dispersion medium. The relative change in the average value was calculated based on the particle size measurement results.

[0179] As shown in Figures 17 to 19, the dry emulsions of Examples 2-1 to 2-3 exhibited the best storage stability at all temperatures, and the dry emulsions of Examples 2-4 to 2-5 exhibited relatively good storage stability, although lower than the dry emulsions of Examples 2-1 to 2-3.

[0180] Through the above results, it was confirmed that the dry emulsion containing the solid nano core containing a high content of ceramide according to the present invention exhibits excellent physical stability of the particles even under various temperature conditions.

Claims

1. A solid nanocore containing ceramide and oleic acid; and Comprising wall materials comprising gum arabic and maltodextrin; A dry emulsion comprising a solid nano core containing a high content of ceramide in powdered form through spray drying.

2. In paragraph 1, The above solid nano cores are, A dry emulsion comprising a solid nano core containing a high content of ceramide, characterized in that ceramide is dissolved in oleic acid and then solidified by adding polysorbate.

3. In paragraph 2, The above oleic acid, A dry emulsion comprising a solid nano core containing a high content of ceramide, characterized in that it is heated to a temperature of 65 to 95 ° C.

4. In paragraph 1, The above ceramides are, A dry emulsion comprising a solid nano core having a high content of ceramide, characterized in that the solid nano core is contained in an amount of 15 to 23 parts by weight based on 100 parts by weight of the dry emulsion.

5. In paragraph 2, The above polysorbate is, A dry emulsion comprising a solid nano core having a high content of ceramide, characterized in that 1 to 1.5 parts by weight are added relative to 1 part by weight of the oleic acid.

6. In paragraph 1, The above solid nano cores are, A dry emulsion comprising a solid nanocore containing a high content of ceramide, characterized by a size of 100 to 300 nm.

7. In paragraph 1, The above wall is, A dry emulsion comprising a solid nano core containing a high content of ceramide, characterized in that the gum arabic and the maltodextrin are mixed in a weight ratio of (4 to 2):

1.

8. In paragraph 1, The above dry emulsion, A dry emulsion comprising a solid nano core containing a high content of ceramide, characterized in that the particle size is 2 to 12 ㎛.

9. In paragraph 1, The above dry emulsion, A dry emulsion comprising a solid nanocore containing a high content of ceramide, characterized by an average particle size of 4 to 8 ㎛.

10. Step of heating oleic acid; A step of dissolving ceramide in the heated high-temperature oleic acid; A step of forming a nano core by adding polysorbate to oleic acid containing the dissolved ceramide; A step of cooling and solidifying the above nano core; Step of mixing Arabic gum and maltodextrin; A step of forming a wall by adding the mixed gum Arabic and maltodextrin onto the solidified nano core; A method for producing a dry emulsion comprising solid nano cores having a high content of ceramide, comprising the step of spray-drying the solid nano cores on which the above-mentioned wall body is formed to produce a powdered dry emulsion.

11. In paragraph 10, The step of heating the above oleic acid is: A method for producing a dry emulsion comprising a solid nano core containing a high content of ceramide, characterized by heating at a temperature of 65 to 95° C.

12. In paragraph 10, The step of dissolving the above ceramide is: A method for producing a dry emulsion comprising a solid nanocore having a high ceramide content, characterized in that the ceramide is dissolved in a concentration of 350 to 550 mg / mL.

13. In paragraph 10, The step of dissolving the above ceramide is: A method for producing a dry emulsion comprising a solid nano core having a high content of ceramide, characterized in that 15 to 23 parts by weight are dissolved relative to 100 parts by weight of the dry emulsion.

14. In paragraph 10, The step of forming the above nano core is: A step of adding oleic acid containing the ceramide and the polysorbate to a solvent heated to a temperature of 65 to 95 ℃; A step of stirring the above mixed solution; and A method for producing a dry emulsion comprising solid nano cores containing a high content of ceramide, characterized by comprising a step of homogenizing the stirred mixed solution by ultrasonic treatment.

15. In paragraph 14, The step of adding oleic acid containing the above ceramide and the above polysorbate is, A method for producing a dry emulsion including a solid nano core containing a high content of ceramide, characterized in that the above oleic acid and the above polysorbate are added in a weight ratio of 1: (1 to 1.5).

16. In paragraph 10, The step of cooling and solidifying the above nano core is: A method for producing a dry emulsion comprising a solid nano core having a high content of ceramide, characterized in that the solidification is achieved by cooling and stabilizing at 2 to 6° C.

17. In paragraph 10, The step of mixing the above gum arabic and maltodextrin is: A method for producing a dry emulsion including a solid nano core containing a high content of ceramide, characterized by mixing the gum arabic and the maltodextrin in a weight ratio of (4 to 2):

1.

18. In paragraph 10, The step of forming the above wall is: A method for producing a dry emulsion comprising solid nano cores having a high ceramide content, characterized by adding 10 to 20 parts by weight of a mixture of gum arabic and maltodextrin relative to 100 parts by weight of the solidified nano cores.

19. In paragraph 10, The step of manufacturing a powdered dry emulsion by spray drying is as follows: 160 to 200 ℃, 0.3 to 0.6 m 2 A method for producing a dry emulsion containing solid nano cores having a high content of ceramide, characterized by spray drying by atomizing at a blowing speed of / min and a pressure of (13 to 15) × 10 kPa.

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