CN115381742A - Cordycepin multiple emulsion, hydrogel ball and preparation method - Google Patents
Cordycepin multiple emulsion, hydrogel ball and preparation method Download PDFInfo
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- KQLDDLUWUFBQHP-UHFFFAOYSA-N Cordycepin Natural products C1=NC=2C(N)=NC=NC=2N1C1OCC(CO)C1O KQLDDLUWUFBQHP-UHFFFAOYSA-N 0.000 title claims abstract description 105
- OFEZSBMBBKLLBJ-BAJZRUMYSA-N cordycepin Chemical compound C1=NC=2C(N)=NC=NC=2N1[C@@H]1O[C@H](CO)C[C@H]1O OFEZSBMBBKLLBJ-BAJZRUMYSA-N 0.000 title claims abstract description 105
- OFEZSBMBBKLLBJ-UHFFFAOYSA-N cordycepine Natural products C1=NC=2C(N)=NC=NC=2N1C1OC(CO)CC1O OFEZSBMBBKLLBJ-UHFFFAOYSA-N 0.000 title claims abstract description 105
- 239000000839 emulsion Substances 0.000 title claims abstract description 82
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- 238000002360 preparation method Methods 0.000 title claims description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 36
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- VBICKXHEKHSIBG-UHFFFAOYSA-N 1-monostearoylglycerol Chemical compound CCCCCCCCCCCCCCCCCC(=O)OCC(O)CO VBICKXHEKHSIBG-UHFFFAOYSA-N 0.000 claims abstract description 19
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- ZEMPKEQAKRGZGQ-AAKVHIHISA-N 2,3-bis[[(z)-12-hydroxyoctadec-9-enoyl]oxy]propyl (z)-12-hydroxyoctadec-9-enoate Chemical compound CCCCCCC(O)C\C=C/CCCCCCCC(=O)OCC(OC(=O)CCCCCCC\C=C/CC(O)CCCCCC)COC(=O)CCCCCCC\C=C/CC(O)CCCCCC ZEMPKEQAKRGZGQ-AAKVHIHISA-N 0.000 claims 1
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Images
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Abstract
The invention provides a cordycepin multiple emulsion, which is W/O/W type, wherein the inner water phase of the cordycepin multiple emulsion is a cordycepin aqueous solution, the oil phase of the cordycepin multiple emulsion is macadamia nut oil and glycerin monostearate, and the outer water phase of the cordycepin multiple emulsion is deionized water; the macadamia nut oil comprises, by mass, 10-25% of macadamia nut oil, 0.5-5% of glyceryl monostearate, 0.5-3% of polyglycerol ricinoleate, 0.1-0.5% of cordycepin, 2-5% of sodium caseinate, 10-20% of internal phase deionized water and the balance of external phase deionized water. The relatively stable cordycepin multiple emulsion is encapsulated in the hydrogel ball, so that the stability of the cordycepin multiple emulsion is further improved. The moisturizing and skin adhesion properties of the hydrogel synergistically enhance the skin absorption of the active ingredient with the cordycepin multiple emulsion.
Description
Technical Field
The invention relates to the technical field of skin care compositions, and particularly relates to a cordycepin multiple emulsion, a hydrogel ball and a preparation method thereof.
Background
Cordycepin is one of active ingredients of Cordyceps sinensis, has antioxidant bioactivity, and has great development and utilization values. At present, researchers mainly apply cordycepin to medicines and foods, and the application of cordycepin to cosmetics is only reported. The antioxidant bioactivity of cordycepin also has a wide application prospect in the aspect of skin care.
Cordycepin has poor lipid solubility, is not easy to be absorbed by human body, has low bioavailability, and limits the application of cordycepin. At present, the carrier technology is generally adopted to improve the bioavailability of active ingredients. Researchers at home and abroad mainly adopt carrier modes such as liposome, high molecular polymer carrier, layered hydroxide cordycepin derivative and the like to be applied to the fields of food and medicine at present.
The water-soluble cordycepin is difficult to permeate the stratum corneum barrier of the skin, if the cordycepin is directly added into the skin care product, most of the cordycepin only stays on the surface of the skin and cannot enter the endothelial layer to exert the effect, so the skin has low absorption rate of the cordycepin if the cordycepin is directly added into the skin care product. At present, the cordycepin is applied to the field of cosmetics, O/W and W/O type emulsions are mostly prepared by emulsification, and the application of cordycepin multiple emulsion hydrogel balls to the cosmetics is not reported.
The multiple emulsion has the advantages of unique two-film three-phase structure, and can be used for coating active ingredients and carriers for drug delivery. The W/O/W type multiple emulsion can eliminate the defects of poor skin moistening effect and greasy use feeling of O/W and W/O type emulsions commonly used in the prior cosmetics, has good cleaning effect, and has good moistening and spreading properties. The multiple emulsion can encapsulate the water-soluble active ingredient in the internal water phase, can encapsulate the oil-soluble active ingredient in the oil phase, and after the effective active ingredient is added in the internal phase, the multiple structure of the multiple emulsion can protect and isolate the internal active ingredient, can delay the release of the active substance, and has wide application prospect in the field of cosmetics.
However, the multiple emulsions have poor stability and easily broken structures, which results in leakage of the active ingredient, and the advantage of using multiple emulsion entrapments is lost. Many methods have been used in some studies to enhance the stability of multiple emulsions, and the common methods are classified into increasing the viscosity of the internal water phase, increasing the viscosity of the external water phase, increasing the thickness of the oil phase, improving the formulation, improving the preparation process, and so on.
The hydrogel is a dispersion with a three-dimensional space network structure formed by physically or chemically crosslinking a high-molecular polymer by taking water as a dispersion medium. Since the hydrogel has a plurality of excellent properties such as high water content, soft texture, good biocompatibility, safety, no toxicity and the like, the hydrogel is widely researched as a delivery carrier of active ingredients in the fields of food, medicine, cosmetics and the like. The hydrogel is usually in the form of hydrogel spheres and has the advantages of simple operation, good repeatability, easy industrial production and the like. The hydrogel ball-encapsulated micro-nano carrier has high application value for improving the stability of the micro-nano carrier and active ingredients and realizing controlled release and targeted drug delivery of the drug. However, few studies have been reported to use hydrogel spheres to encapsulate multiple emulsions and their use on topical skin.
In order to improve the stability and the percutaneous absorption rate of cordycepin, the invention provides a cordycepin multiple emulsion hydrogel ball which has wide application prospect in the field of cosmetic production and preparation.
Disclosure of Invention
The invention aims to provide a cordycepin multiple emulsion, a hydrogel ball and a preparation method thereof, so as to solve the technical problems.
In order to achieve the purpose, the invention provides a cordycepin multiple emulsion which is W/O/W type, wherein the inner water phase of the cordycepin multiple emulsion is cordycepin aqueous solution, the oil phase is macadamia nut oil and glycerin monostearate, and the outer water phase is deionized water; the macadamia nut oil comprises, by mass, 10-25% of macadamia nut oil, 0.5-5% of glyceryl monostearate, 0.5-3% of polyglycerol ricinoleate, 0.1-0.5% of cordycepin, 2-5% of sodium caseinate, 10-20% of internal phase deionized water and the balance of external phase deionized water. The polyglycerol polyricinoleate is a water-in-oil emulsifier for promoting the stability of the water phase and the oil phase of the inner layer; the sodium caseinate is an oil-in-water emulsifier for promoting the stability of the outer water phase and the outer oil phase; cordycepin is used as active ingredient; the inner phase deionized water refers to deionized water in the inner phase of the cordycepin multiple emulsion; the external phase deionized water refers to deionized water in the external phase of the cordycepin multiple emulsion.
The preparation method of the cordycepin multiple emulsion is a two-step emulsification method, and comprises the following steps:
step S01: dissolving cordycepin in internal phase deionized water to obtain cordycepin aqueous solution; mixing the cordycepin aqueous solution, the macadamia nut oil, the glyceryl monostearate and the polyglycerol ricinoleate, and stirring and emulsifying at 60-70 ℃ to obtain a W/O type primary emulsion;
step S02: dissolving sodium caseinate in external phase deionized water to obtain a sodium caseinate aqueous solution; and slowly dripping the primary emulsion obtained in the step S01 into an aqueous solution of sodium caseinate, and stirring and emulsifying at the temperature of 45 to 55 ℃ to obtain the W/O/W type cordycepin multiple emulsion.
Further, the rotation speed of stirring and emulsifying in the step S01 is 550 to 650r/min; the stirring time is 10 to 20min.
Further, the rotation speed of stirring and emulsifying in the step S02 is 350 to 450r/min; the stirring time is 5 to 15min.
In order to improve the stability of the cordycepin multiple emulsion, the cordycepin multiple emulsion can be further prepared into hydrogel balls; the method for preparing the hydrogel spheres comprises the following steps: mixing the cordycepin multiple emulsion with chitosan hydrogel with the concentration of 1 to 6% according to the mass ratio of 1 to 0.8 to 1.2, uniformly stirring, dropwise adding into a sodium tripolyphosphate aqueous solution with the mass percentage of 1 to 3%, crosslinking, and washing with deionized water to obtain a hydrogel ball.
The cordycepin multiple emulsion and the application of the hydrogel spheres prepared from the cordycepin multiple emulsion in the field of cosmetic skin care.
Has the advantages that:
(1) The W/O/W type multiple emulsion can make up the defects of O/W and W/O type emulsions, has excellent service performance, high-efficiency cleaning effect, excellent lubricating effect and less greasy feeling, and can play a good role in protecting the active ingredients of the water-soluble cordycepin added in the internal phase due to the unique multiple structure.
(2) The cordycepin multiple emulsion can also control the release time of the cordycepin active ingredient, and has slow release or quick release effect under certain conditions.
(3) The relatively stable cordycepin multiple emulsion is encapsulated in the hydrogel ball, so that the stability of the cordycepin multiple emulsion is further improved.
(4) The moisturizing and skin adhesion properties of the hydrogel synergistically enhance the skin absorption of the active ingredient with the cordycepin multiple emulsion.
(5) The hydrogel adopted by the invention is edible type of natural polymer, the emulsifier is edible type, and the product is healthy and environment-friendly.
Drawings
Fig. 1 is a structural diagram of the morphology of cordycepin multiple emulsion hydrogel spheres observed in test example 1.
FIG. 2 is a graph showing the comparison results of 24h permeation rates of cordycepin in skin by the cordycepin aqueous solution, the cordycepin multiple emulsion and the cordycepin multiple emulsion hydrogel spheres in comparative example 1.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings of the present invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention. Unless defined otherwise, technical or scientific terms used herein shall have the ordinary meaning as understood by one of ordinary skill in the art to which this invention belongs. As used herein, the word "comprising" and similar words are intended to mean that the element or item preceding the word comprises the element or item listed after the word and its equivalent, but not the exclusion of other elements or items.
Aiming at the problems in the prior art, the embodiment of the invention provides a cordycepin multiple emulsion, a hydrogel ball and a preparation method.
Example 1
Preparing a cordycepin aqueous solution with the mass percentage (wt%) of 2%, weighing 3.5g of the cordycepin aqueous solution, 5.0g of macadamia nut oil, 1.0g of glyceryl monostearate and 0.5g of polyglycerol ricinoleate into a reaction bottle, placing the reaction bottle into a constant-temperature water bath kettle, and magnetically stirring for 15min at the constant temperature of 65 ℃ and the rotating speed of 600 r/min until the components are uniformly mixed to obtain a primary emulsion;
preparing a 5 wt% sodium caseinate aqueous solution, wherein the mass ratio of the primary emulsion to the sodium caseinate aqueous solution is 1.
Mixing the prepared cordycepin multiple emulsion with chitosan hydrogel with the concentration of 3% according to the mass ratio of 1.
And (3) performance detection results: after the prepared cordycepin multiple emulsion hydrogel balls are stored for 6 months at 25 ℃, the retention rate of cordycepin is 65 percent, and the percutaneous absorption rate is 12 percent.
Example 2
Preparing a cordycepin aqueous solution with the mass percentage (wt%) of 2%, weighing 4.0g of the cordycepin aqueous solution, 5.0g of macadamia nut oil, 0.6g of glyceryl monostearate and 0.4g of polyglycerol ricinoleate into a reaction bottle, placing the reaction bottle in a constant-temperature water bath kettle, and magnetically stirring at the constant temperature of 65 ℃ and the rotating speed of 600 r/min for 15min until the components are uniformly mixed to obtain a primary emulsion; 3.5
Preparing a 5 wt% sodium caseinate aqueous solution, wherein the mass ratio of the primary emulsion to the sodium caseinate aqueous solution is 1.
Mixing the prepared cordycepin multiple emulsion with 5% chitosan hydrogel according to a mass ratio of 1.
And (3) performance detection results: after the prepared cordycepin multiple emulsion hydrogel balls are stored for 6 months at 25 ℃, the retention rate of cordycepin is 68 percent, and the percutaneous absorption rate is 13 percent.
Example 3
Preparing a cordycepin aqueous solution with the mass percentage (wt%) of 2%, weighing 4.5g of the cordycepin aqueous solution, 5.0g of macadamia nut oil, 0.3g of glyceryl monostearate and 0.2g of polyglycerol ricinoleate into a reaction bottle, placing the reaction bottle into a constant-temperature water bath kettle, and magnetically stirring for 15min at the constant temperature of 65 ℃ and the rotating speed of 600 r/min until the components are uniformly mixed to obtain a primary emulsion;
preparing a 5 wt% sodium caseinate aqueous solution, wherein the mass ratio of the primary emulsion to the sodium caseinate aqueous solution is 1.
Mixing the prepared cordycepin multiple emulsion with 4% chitosan hydrogel according to a mass ratio of 1.
And (3) performance detection results: after the prepared cordycepin multiple emulsion hydrogel spheres are stored for 6 months at 25 ℃, the retention rate of cordycepin is 60 percent, and the percutaneous absorption rate is 10 percent.
Test example 1
Observing the morphological structure of the cordycepin multiple emulsion hydrogel spheres prepared in the example 2 by a common optical microscope; placing the cordycepin multiple emulsion hydrogel ball prepared in the embodiment 2 on a glass slide, covering a cover glass, slightly pressing, and observing the inner edge of the cordycepin multiple emulsion hydrogel ball through an optical microscope; the observation results are shown in FIG. 1.
Comparative example 1
The transdermal behavior of cordycepin in the cordycepin aqueous solution, the cordycepin multiple emulsion and the cordycepin multiple emulsion hydrogel spheres in the example 2 is evaluated by adopting a vertical Franz diffusion cell method, and the transdermal diffusion instrument is used for detecting the permeability of cordycepin in the skin within 24 hours; the results of the experiment are shown in FIG. 2.
The experimental result shows that compared with the cordycepin aqueous solution, the cordycepin multiple emulsion has obviously improved permeability within 24 hours of cordycepin in the skin. Compared with cordycepin multiple emulsion hydrogel balls, the cordycepin multiple emulsion hydrogel balls have the advantage that the permeability of cordycepin in skin within 24 hours is further improved. Hydrogels can enhance the penetration of actives by moisturizing and increasing the hydration of the skin.
Although the embodiments of the present invention have been described in detail hereinabove, it is apparent to those skilled in the art that various modifications and variations can be made to these embodiments. However, it is to be understood that such modifications and variations are within the scope and spirit of the present invention as set forth in the following claims. Moreover, the invention as described herein is capable of other embodiments and of being practiced or of being carried out in various ways.
Claims (7)
1. The cordycepin multiple emulsion is characterized by being W/O/W type, the inner water phase of the cordycepin multiple emulsion is a cordycepin aqueous solution, the oil phase of the cordycepin multiple emulsion is macadamia nut oil and glycerin monostearate, and the outer water phase of the cordycepin multiple emulsion is deionized water; the macadamia nut oil cleaning agent comprises, by mass, 10-25% of macadamia nut oil, 0.5-5% of glyceryl monostearate, 0.5-3% of polyglycerol ricinol, 0.1-0.5% of cordycepin, 2-5% of sodium caseinate, 10-20% of internal phase deionized water and the balance external phase deionized water.
2. The method for preparing the cordycepin multiple emulsion according to claim 1, wherein the method for preparing the cordycepin multiple emulsion is a two-step emulsification method, comprising the following steps:
step S01: dissolving cordycepin in internal phase deionized water to obtain cordycepin aqueous solution; mixing the cordycepin aqueous solution, the macadamia nut oil, the glyceryl monostearate and the polyglycerol ricinoleate, and stirring and emulsifying at 60 to 70 ℃ to obtain a W/O type primary emulsion;
step S02: dissolving sodium caseinate in external deionized water to obtain sodium caseinate aqueous solution; and slowly dripping the primary emulsion obtained in the step S01 into an aqueous solution of sodium caseinate, and stirring and emulsifying at the temperature of 45 to 55 ℃ to obtain the W/O/W type cordycepin multiple emulsion.
3. The method for preparing the cordycepin multiple emulsion according to claim 2, wherein the rotation speed of stirring and emulsifying in the step S01 is 550 to 650r/min; the stirring time is 10 to 20min.
4. The preparation method of the cordycepin multiple emulsion according to claim 2, wherein the rotation speed of stirring and emulsifying in the step S02 is 350 to 450r/min; the stirring time is 5 to 15min.
5. Hydrogel spheres prepared from the cordycepin multiple emulsion of claim 1.
6. The method for preparing hydrogel spheres from the cordycepin multiple emulsion of claim 1, wherein the method for preparing hydrogel spheres comprises the following steps: mixing the cordycepin multiple emulsion and the chitosan hydrogel with the concentration of 1-6% according to the mass ratio of 1: 0.8-1.2, stirring uniformly, then dropwise adding the mixture into a sodium tripolyphosphate aqueous solution with the mass percentage of 1-3% for crosslinking, and washing with deionized water to obtain the hydrogel sphere.
7. The cordycepin multiple emulsion as claimed in claim 1 or 5 and application of hydrogel spheres prepared from the cordycepin multiple emulsion in the field of cosmetic skin care.
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