CN110974711A - Azelaic acid microcapsule and preparation method thereof - Google Patents
Azelaic acid microcapsule and preparation method thereof Download PDFInfo
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- CN110974711A CN110974711A CN201911265889.5A CN201911265889A CN110974711A CN 110974711 A CN110974711 A CN 110974711A CN 201911265889 A CN201911265889 A CN 201911265889A CN 110974711 A CN110974711 A CN 110974711A
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/30—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
- A61K8/33—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing oxygen
- A61K8/36—Carboxylic acids; Salts or anhydrides thereof
- A61K8/362—Polycarboxylic acids
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/02—Cosmetics or similar toiletry preparations characterised by special physical form
- A61K8/11—Encapsulated compositions
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/92—Oils, fats or waxes; Derivatives thereof, e.g. hydrogenation products thereof
- A61K8/922—Oils, fats or waxes; Derivatives thereof, e.g. hydrogenation products thereof of vegetable origin
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
- A61Q19/00—Preparations for care of the skin
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
- A61Q19/00—Preparations for care of the skin
- A61Q19/02—Preparations for care of the skin for chemically bleaching or whitening the skin
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2800/00—Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
- A61K2800/74—Biological properties of particular ingredients
- A61K2800/78—Enzyme modulators, e.g. Enzyme agonists
- A61K2800/782—Enzyme inhibitors; Enzyme antagonists
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Abstract
The invention discloses a azelaic acid microcapsule and a preparation method thereof, belonging to the technical field of microcapsules; the microcapsule consists of two parts, namely a wall material and a core material, wherein the wall material adopts inorganic material calcium carbonate, the core material adopts azelaic acid with whitening, freckle removing and acne removing functions and jasmine essential oil with the functions of increasing skin elasticity and making the skin tender, and the mass ratio of the core material to the wall material is 1 (4-9). The microcapsule prepared by the invention can realize the effective utilization of azelaic acid and the absorption of human skin, greatly improve the stability and compatibility of azelaic acid, and has great development prospect in the fields of acne removing, freckle removing, whitening and the like.
Description
Technical Field
The invention belongs to the field of microcapsules, and particularly relates to a microcapsule with effects of whitening, removing acnes and freckles and a preparation method thereof.
Background
Azelaic acid, also known as azelaic acid, a naturally occurring natural straight chain saturated carboxylic acid containing 9 carbon atoms, an important chemical raw material, has high value in the aspects of skin care, beauty and prevention and treatment of skin diseases, and firstly can competitively inhibit tyrosinase, whiten skin and remove color spots; the other purpose is bacteriostasis, and the azelaic acid can inhibit the protein synthesis of cells and has inhibition effect on staphylococcus, acne propionic acid bacteria, escherichia coli and the like; in addition, azelaic acid can inhibit the secretion of free fatty acids in sebaceous glands and regulate the normal secretion of sebum, so that azelaic acid can also be used for treating acne. However, the azelaic acid has poor compatibility, poor water solubility, easy color change, difficult dissolution, poor stability when being used in cosmetics and poor spreadability, and when the azelaic acid is dissolved in an unconventional manner, the content of the azelaic acid can be reduced, even the using effect can be reduced, so that the application of the azelaic acid in the cosmetics is greatly limited.
The jasmine essential oil is called as the king of essential oil, not only has elegant fragrance, but also can care and improve the conditions of dry skin, water shortage, oil passing and sensitivity, fade scars, increase skin elasticity, delay skin aging and make the skin tender.
Microencapsulation is an emerging technology, which is a technology that allows the release of a solid, liquid or gas at a controlled rate under specific conditions, typically in the range of 5-200 μm, by embedding it in a small, sealed capsule. For substances which have large irritation to human skin and poor solubility in cosmetics, the substances can be wrapped in corresponding wall materials through a microencapsulation technology to play a role in slow release and be better absorbed by human bodies; meanwhile, the solubility of the substance is greatly improved, so that the substance is more widely applied to cosmetics; the technology also avoids the influence of light, heat and oxygen on the active components, and plays a certain role in protecting the active components. The prior literature reports a few applications of azelaic acid in cosmetics and exists mainly as azelaic acid derivative (K-ADG), which is a potassium salt prepared by reacting azelaic acid with amino acids.
Disclosure of Invention
The invention aims to provide a substance microcapsule with whitening, acne removing and freckle removing functions and a preparation method thereof, and the preparation method can effectively solve the problems of poor stability and poor solubility of azelaic acid.
In order to achieve the above object, the present invention provides an azelaic acid microcapsule, which is characterized in that calcium carbonate is used as a wall material, azelaic acid is used as a core material, and the mass ratio of the core material is as follows: the wall material is 1 (4-9).
The invention also provides a preparation method of the azelaic acid microcapsule, which is characterized by comprising the following steps:
1) dissolving azelaic acid in jasmine essential oil, carrying out constant-temperature water bath at 30-45 ℃ and 400-500 r/min, and stirring to obtain azelaic acid solution, wherein the mass ratio of the azelaic acid to the jasmine essential oil is 1 (5-10);
2) dissolving Tween-20 in deionized water, stirring for 10-15 min at the speed of 400-500 r/min in a constant-temperature water bath at the temperature of 30-45 ℃, adding the mixture into the azelaic acid solution obtained in the step 1), and continuously stirring for 10-15 min to form a core material solution, wherein the mass ratio of Tween to deionized water is (0.5-1): 100;
3) dissolving calcium chloride in deionized water, stirring at the rotating speed of 400-700 r/min, controlling the temperature to be 30-45 ℃, dropwise adding the obtained calcium chloride solution into the core material solution prepared in the step 2), and continuously stirring for 1.5-2 hours to obtain a precursor solution;
4) and (2) dissolving sodium carbonate into deionized water, wherein the mass ratio of the sodium carbonate to the water is (7.6-9.5): 50, dropwise adding the sodium carbonate to the precursor solution prepared in the step 3), stirring for 2-3 h, standing for 18-36 h, carrying out suction filtration and drying to obtain the azelaic acid microcapsule.
Preferably, the mass ratio of the azelaic acid to the Tween-20 is (2-4): 1.
Preferably, the mass ratio of the azelaic acid to the calcium chloride is 1 (4-10).
Preferably, the mass ratio of the calcium chloride to the sodium carbonate is 1 (0.95-0.96).
Compared with the prior art, the invention has the beneficial effects that:
(1) the microcapsule containing azelaic acid obtained by the invention has the advantages that the stability is obviously improved by adopting a microcapsule technology, the release speed of the active component is maintained in a stable state, so that the damage to skin caused by excessive local dosage is prevented, the service life is prolonged, and the microcapsule exists in a microcapsule form and is more beneficial to skin absorption. It is excellent for application or absorption in cosmetics.
(2) The microcapsule containing azelaic acid obtained by the invention is formed by adopting a microcapsule technology, so that the stability is excellent, and the preparation method is simple and convenient. In the form of microcapsule, the light stability, thermal stability and compatibility of oil phase raw materials are improved, the compatibility of azelaic acid is also improved, and the obtained type of azelaic acid microcapsule forms a functional material, has white powder appearance and strong stability.
(3) Because the natural jasmine essential oil is adopted, the jasmine essential oil is remarkable in nursing and improving skin dryness, fading scars and increasing skin elasticity. The invention better combines the jasmine essential oil with the azelaic acid, recycles the jasmine essential oil on the skin, expands the application value of the azelaic acid and has wider application range.
Detailed Description
The invention will be further illustrated with reference to the following specific examples. It should be understood that these examples are for illustrative purposes only and are not intended to limit the scope of the present invention. Further, it should be understood that various changes or modifications of the present invention may be made by those skilled in the art after reading the teaching of the present invention, and such equivalents may fall within the scope of the present invention as defined in the appended claims.
The specification of various raw materials or reagents used in the invention and the information of manufacturers are as follows:
name of reagent | Specification of | Manufacturer of the product |
Azelaic acid | Analytical purity | Chemical reagents of national drug group Co Ltd |
Sodium carbonate | Analytical purity | Chemical reagents of national drug group Co Ltd |
Tween-20 | Analytical purity | Chemical reagents of national drug group Co Ltd |
Calcium chloride | Analytical purity | Chemical reagents of national drug group Co Ltd |
Jasmine essential oil | --- | Shanghai Ixocetin perfumes Co Ltd |
Some of the instrument manufacturers and models used in the invention are as follows:
example 1
The embodiment provides an azelaic acid microcapsule, which takes inorganic material calcium carbonate as a wall material and azelaic acid as a core material, and the mass ratio of the core material is as follows: the wall material is 1: 9;
the preparation method of the azelaic acid microcapsule specifically comprises the following steps:
1) putting 1g of azelaic acid and 10g of jasmine essential oil into a beaker, and putting the beaker into a constant-temperature water bath kettle at the temperature of 45 ℃ to stir at the speed of 400r/min to obtain an azelaic acid solution;
2) dissolving 0.5g of Tween-20 in 10ml of deionized water, stirring for 10min at the speed of 500r/min in a constant-temperature water bath at 45 ℃, adding into the solution obtained in the step 1), and continuously stirring for 10min to form a core material solution;
3) weighing 9G of calcium chloride, dissolving in 50ml of deionized water, and stirring by using a 524G type magnetic stirrer at a rotating speed of 600r/min to uniformly disperse the calcium chloride in the deionized water;
4) controlling the dropping speed to be 1ml/min, dropwise adding the calcium chloride solution obtained in the step 3) into the core material solution prepared in the step 2), controlling the temperature to be 45 ℃, and continuously stirring for 2 hours after dropwise adding is finished;
5) weighing 8.6G of sodium carbonate, dissolving in 50ml of deionized water, and stirring by using a 524G type magnetic stirrer at the rotating speed of 600r/min to uniformly disperse the sodium carbonate in the deionized water to obtain a sodium carbonate solution;
6) dropwise adding the sodium carbonate solution obtained in the step 5) into the sodium carbonate solution obtained in the step 4) at a concentration of 1ml/min, controlling the temperature to be 45 ℃, stirring for 2 hours after dropwise adding, and standing for 24 hours;
7) and (3) carrying out suction filtration on the solution obtained in the step 6) by using a circulating water type multipurpose vacuum pump, and drying by using a 101 type digital display air-blast drying oven at 50 ℃ to obtain white powdery microcapsules.
The obtained azelaic acid microcapsule has the yield of 56.7 percent, is white powder, has soft jasmine fragrance, greatly improves the compatibility and stability, is suitable for being used in skin care products, has the effects of whitening, removing acne, removing freckles and the like, can play a role of slow release when being acted on the skin, reduces the stimulation caused by directly acting on the skin, and exists in a stable form.
example 2
The embodiment provides an azelaic acid microcapsule, which takes inorganic material calcium carbonate as a wall material and azelaic acid as a core material, and the mass ratio of the core material is as follows: the wall material is 2: 8;
the preparation method of the azelaic acid microcapsule specifically comprises the following steps:
1) putting 2g of azelaic acid and 14g of jasmine essential oil into a beaker, and putting the beaker into a constant-temperature water bath kettle at the temperature of 45 ℃ to stir at the speed of 400r/min to obtain an azelaic acid solution;
2) dissolving 0.5g of Tween-20 in 10ml of deionized water, stirring for 10min at the speed of 500r/min in a constant-temperature water bath at 45 ℃, adding into the solution obtained in the step 1), and continuously stirring for 10min to form a core material solution;
3) weighing 8G of calcium chloride, dissolving the calcium chloride in 50ml of deionized water, and stirring the calcium chloride by using a 524G type magnetic stirrer at the rotating speed of 600r/min to uniformly disperse the calcium chloride in the deionized water;
4) controlling the dropping speed to be 1ml/min, dropwise adding the calcium chloride solution obtained in the step 3) into the core material solution prepared in the step 2), controlling the temperature to be 45 ℃, and continuously stirring for 2 hours after dropwise adding is finished;
5) weighing 7.6G of sodium carbonate, dissolving in 50ml of deionized water, and stirring by using a 524G type magnetic stirrer at the rotating speed of 600r/min to uniformly disperse the sodium carbonate in the deionized water to obtain a sodium carbonate solution;
6) dropwise adding the sodium carbonate solution obtained in the step 5) into the sodium carbonate solution obtained in the step 4) at a concentration of 1ml/min, controlling the temperature to be 45 ℃, stirring for 2 hours after dropwise adding, and standing for 24 hours;
7) and (3) carrying out suction filtration on the solution obtained in the step 6) by using a circulating water type multipurpose vacuum pump, and drying by using a 101 type digital display air-blast drying oven at 50 ℃ to obtain white powdery microcapsules.
The yield of the obtained azelaic acid microcapsule is 43.53 percent, the azelaic acid microcapsule has good embedding effect on capsule cores, is white powder, has small particle size, is easy to be absorbed by human bodies, is used as a whitening functional material, meets the requirement of human on deeper skin, cannot cause pore blockage, has simple preparation process, and greatly improves the compatibility and the stability.
example 3
The embodiment provides an azelaic acid microcapsule, which takes inorganic material calcium carbonate as a wall material and azelaic acid as a core material, and the mass ratio of the core material is as follows: the wall material is 2: 10;
the preparation method of the azelaic acid microcapsule specifically comprises the following steps:
1) putting 2g of azelaic acid and 15g of jasmine essential oil into a beaker, and putting the beaker into a constant-temperature water bath kettle at the temperature of 45 ℃ to stir at the speed of 400r/min to obtain an azelaic acid solution;
2) dissolving 0.5g of Tween-20 in 10ml of deionized water, stirring for 10min at the speed of 500r/min in a constant-temperature water bath at 45 ℃, adding into the solution obtained in the step 1), and continuously stirring for 10min to form a core material solution;
3) weighing 10G of calcium chloride, dissolving in 50ml of deionized water, and stirring by using a 524G type magnetic stirrer at a rotating speed of 600r/min to uniformly disperse the calcium chloride in the deionized water;
4) controlling the dropping speed to be 1ml/min, dropwise adding the calcium chloride solution obtained in the step 3) into the core material solution prepared in the step 2), controlling the temperature to be 45 ℃, and continuously stirring for 2 hours after dropwise adding is finished;
5) weighing 9.5G of sodium carbonate, dissolving in 50ml of deionized water, and stirring by using a 524G type magnetic stirrer at the rotating speed of 600r/min to uniformly disperse the sodium carbonate in the deionized water to obtain a sodium carbonate solution;
6) dropwise adding the sodium carbonate solution obtained in the step 5) into the sodium carbonate solution obtained in the step 4) at a concentration of 1ml/min, controlling the temperature to be 45 ℃, stirring for 2 hours after dropwise adding, and standing for 24 hours;
7) and (3) carrying out suction filtration on the solution obtained in the step 6) by using a circulating water type multipurpose vacuum pump, and drying by using a 101 type digital display air-blast drying oven at 50 ℃ to obtain white powdery microcapsules.
The yield of the obtained azelaic acid microcapsule is 57.95%, the azelaic acid microcapsule is white powder, jasmine fragrance is soft, compatibility and stability of the azelaic acid microcapsule are obviously improved compared with those of azelaic acid directly used, and compatibility and stability of azelaic acid in cosmetics are greatly improved.
Claims (5)
1. the azelaic acid microcapsule is characterized in that calcium carbonate is used as a wall material, azelaic acid is used as a core material, and the mass ratio of the core material is as follows: the wall material is 1 (4-9).
2. A process for the preparation of azelaic acid microcapsules according to claim 1, characterized in that it comprises the following steps:
1) dissolving azelaic acid in jasmine essential oil, carrying out constant-temperature water bath at 30-45 ℃ and 400-500 r/min, and stirring to obtain azelaic acid solution, wherein the mass ratio of the azelaic acid to the jasmine essential oil is 1 (5-10);
2) dissolving Tween-20 in deionized water, stirring for 10-15 min at the speed of 400-500 r/min in a constant-temperature water bath at the temperature of 30-45 ℃, adding the mixture into the azelaic acid solution obtained in the step 1), and continuously stirring for 10-15 min to form a core material solution, wherein the mass ratio of Tween to deionized water is (0.5-1): 100;
3) dissolving calcium chloride in deionized water, stirring at the rotating speed of 400-700 r/min, controlling the temperature to be 30-45 ℃, dropwise adding the obtained calcium chloride solution into the core material solution prepared in the step 2), and continuously stirring for 1.5-2 hours to obtain a precursor solution;
4) and (2) dissolving sodium carbonate into deionized water, wherein the mass ratio of the sodium carbonate to the water is (7.6-9.5): 50, dropwise adding the sodium carbonate to the precursor solution prepared in the step 3), stirring for 2-3 h, standing for 18-36 h, carrying out suction filtration and drying to obtain the azelaic acid microcapsule.
3. The method for preparing azelaic acid microcapsules according to claim 2, wherein the mass ratio of azelaic acid to tween-20 is (2-4): 1.
4. The method for preparing azelaic acid microcapsules according to claim 2, wherein the mass ratio of azelaic acid to calcium chloride is 1 (4-10).
5. The method for preparing azelaic acid microcapsules according to claim 2, wherein the mass ratio of calcium chloride to sodium carbonate is 1 (0.95-0.96).
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CN112618420A (en) * | 2021-01-12 | 2021-04-09 | 上海应用技术大学 | Jojoba oil-loaded microcapsule and preparation method thereof |
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