CN117398293A - Preparation method and application of liposome for wrapping soothing and repairing components by using micro-jet homogenizer - Google Patents

Preparation method and application of liposome for wrapping soothing and repairing components by using micro-jet homogenizer Download PDF

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CN117398293A
CN117398293A CN202311263630.3A CN202311263630A CN117398293A CN 117398293 A CN117398293 A CN 117398293A CN 202311263630 A CN202311263630 A CN 202311263630A CN 117398293 A CN117398293 A CN 117398293A
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liposome
micro
extract
ceramide
soothing
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CN117398293B (en
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肖建东
黄丽琼
潘武
黄全胜
包计贤
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Haoyu Guangzhou Cosmetics Manufacturing Co ltd
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    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
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    • A61K8/33Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing oxygen
    • A61K8/34Alcohols
    • A61K8/345Alcohols containing more than one hydroxy group
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    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
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    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
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    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/30Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
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    • A61K8/67Vitamins
    • A61K8/678Tocopherol, i.e. vitamin E
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    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/30Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
    • A61K8/68Sphingolipids, e.g. ceramides, cerebrosides, gangliosides
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
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    • A61K8/96Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution
    • A61K8/97Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution from algae, fungi, lichens or plants; from derivatives thereof
    • A61K8/9783Angiosperms [Magnoliophyta]
    • A61K8/9789Magnoliopsida [dicotyledons]
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    • A61K8/9783Angiosperms [Magnoliophyta]
    • A61K8/9794Liliopsida [monocotyledons]
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61QSPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q19/00Preparations for care of the skin
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    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
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    • A61K2800/40Chemical, physico-chemical or functional or structural properties of particular ingredients
    • A61K2800/59Mixtures
    • A61K2800/592Mixtures of compounds complementing their respective functions
    • AHUMAN NECESSITIES
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    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2800/00Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
    • A61K2800/80Process related aspects concerning the preparation of the cosmetic composition or the storage or application thereof
    • A61K2800/82Preparation or application process involves sonication or ultrasonication

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Abstract

The invention relates to a preparation method and application of liposome for wrapping a soothing and repairing component by using a micro-jet homogenizer. The ceramide NP in the liposome prepared by the process is uniformly dispersed and can be stably present in the liposome; the preparation method does not contain solubilizer, preservative and permeation aid, and the obtained liposome is bubble-free and has the effects of nano particle size, strong efficacy, good absorption, low irritation and good stability; the preparation method enables the effects of various soothing components, moisturizing, repairing and maintaining active components such as skin to be better exerted, and endows the liposome with excellent effects of soothing skin, moisturizing, repairing and maintaining skin.

Description

Preparation method and application of liposome for wrapping soothing and repairing components by using micro-jet homogenizer
Technical Field
The invention relates to the technical field of liposome preparation, in particular to a preparation method and application of liposome for wrapping a soothing and repairing component by using a micro-jet homogenizer
Background
Liposome technology is a method used in the cosmetic industry for encapsulation, preservation and controlled release of bioactive components. Liposomes are spherical vesicles consisting of a phospholipid bilayer and a water core, and can range in size from nano-scale to micro-scale. Liposome technology can increase the permeability of low-permeability and low-water-solubility active ingredients on the skin, on one hand, because the phospholipid bilayer membrane of the liposome has components and structures similar to cell membranes, and is easy to reach deep skin through intercellular lipids, and on the other hand, because the charge on the surface of the liposome can interact with the skin to help the active ingredients to increase the permeability.
Ceramide NPs are relatively poorly soluble in water and oil, and their use in traditional cosmetics is difficult. And compared with the liposome, the traditional cosmetic has the defects that the ceramide NP is added to the liposome, crystals are easy to be separated out, and the skin absorption effect is relatively insufficient.
Based on the above, the invention provides a preparation method for preparing liposome for wrapping soothing and repairing components by using a micro-jet homogenizer, which aims to solve the problems of poor solubility, instability, poor compatibility effect, strong irritation and poor skin absorption effect of liposome active components.
Disclosure of Invention
The invention is based on the solution of the technical problems, thereby providing a preparation method and application of liposome for wrapping the soothing and repairing component by using a micro-jet homogenizer, and ceramide NP in the liposome prepared by the process of the invention is uniformly dispersed and can exist in the liposome stably; the preparation method of the liposome does not contain solubilizer, preservative and permeation aid, and the obtained liposome is bubble-free and has the effects of nano particle size, strong efficacy, good absorption, low irritation and good stability; the preparation method enables the effects of various soothing components, moisturizing, repairing and maintaining active components such as skin to be better exerted, and endows the liposome with excellent effects of soothing skin, moisturizing, repairing and maintaining skin.
In one aspect, the invention provides a method for preparing liposome for wrapping a soothing and repairing component by using a micro-jet homogenizer, which is characterized by comprising the following steps: the method comprises the following steps:
(1) Weighing raw materials: centella asiatica extract complex, dendrobium nobile extract, ceramide NP, stearyl glycyrrhetinate, phosphatidylcholine, cholesterol, phytosphingosine, tocopherol, glycerin, and water; wherein the centella extract complex is a mixture of madecassoside and asiaticoside and centella leaf extract;
pretreatment of raw materials: dissolving ceramide NP, phosphatidylcholine, centella asiatica extract complex, stearyl glycyrrhetinate, cholesterol, phytosphingosine and tocopherol in an organic solvent, performing ultrasonic dissolution, then further uniformly mixing, and then transferring to a rotary evaporator to remove the organic solvent to obtain an oil phase of ceramide NP-phosphatidylcholine-centella asiatica extract complex-stearyl glycyrrhetinate-tocopherol;
(2) Mixing glycerol, herba Dendrobii extract and water to obtain water phase;
(3) Pouring the water phase into the oil phase for mixing, and uniformly stirring to obtain a pre-emulsion;
(4) Homogenizing the pre-emulsion by using a micro-jet homogenizer to obtain the liposome.
Further, the organic solvent in the step (1) comprises at least one of methanol, ethanol, chloroform, ethyl acetate, n-hexane and petroleum ether. Still further is ethanol.
Further, in the step (1), the mass ratio of the sum of ceramide NP, phosphatidylcholine, centella asiatica extract complex, stearyl glycyrrhetinate, cholesterol, phytosphingosine and tocopherol to the organic solvent is 1: (10-100), 1: (15-900), 1: (20-80) or 1: (20-60).
Further, the ultrasound in step (1) is performed at a power of 80W, 160W, 240W or 320W. Further, the ultrasonic time is 2 to 120 minutes, 3 to 100 minutes, 4 to 80 minutes, or 5 to 60 minutes. Further, the ultrasonic frequency is 20-100KHz, 25-90KHz, 30-80KHz or 30-600KHz.
Further, the mixing step of obtaining the oil phase and the water phase in the steps (1) and (2) is carried out under the stirring condition.
Further, the stirring speeds of the mixing steps of the oil phase and the water phase obtained in the steps (1) and (2) are respectively and independently 20-500 rpm, 50-400 rpm or 60-300 rpm.
Further, the stirring time of the mixing step for obtaining the oil phase and the water phase in the steps (1) and (2) is respectively and independently 0.2-5 hours, 0.5-4 hours or 0.6-2 hours.
Further, the stirring temperature of the mixing step of the oil phase and the water phase obtained in the steps (1) and (2) is respectively and independently 20-70 ℃, 25-65 ℃ or 30-60 ℃.
Further, the mixing step in the step (3) is performed under stirring.
Further, the stirring speed in the step (3) is 50-800 rpm, 60-600 rpm or 70-400 rpm.
Further, the stirring time in the step (3) is 0.5-6 hours, 1-5 hours or 1-4 hours.
Further, the stirring temperature in the step (3) is 30-75 ℃, 35-70 ℃ or 40-65 ℃.
Further, the micro-jet homogenizer in the step (4) is a micifuga micro-jet homogenizer.
Further, the micro-jet homogenizer in the step (4) is an MF7250IP-EH production type high-pressure micro-jet homogenizer of Shanghai Miao biosciences Co.
Further, the homogenizing pressure of the microfluidizer in the step (4) is 20-300MPa, 30-250MPa or 50-200MPa.
Further, the homogenizing time of the micro-jet in the step (4) is 2-120min, 2.5-80min or 3-30min.
Further, the preparation raw materials comprise, by mass, 0.1-1% of centella asiatica extract complex, 0.1-1% of dendrobium nobile extract, 0.1-2% of ceramide NP, 0.1-1% of stearyl glycyrrhetinate, 0.1-10% of phosphatidylcholine, 0.1-5% of cholesterol, 0.1-5% of phytosphingosine, 0.1-1% of tocopherol, 20-60% of glycerol and 14-75% of water; wherein, the centella extract compound comprises the following components in mass ratio of 50:15:35 madecassoside, asiaticoside and centella asiatica leaf extract.
Further, the centella asiatica extract complex is used in a mass percent amount of 0.2, 0.4, 0.5, 0.7, 0.8, 0.9 or any two ranges of values.
Further, the dendrobium nobile extract is used in a mass percentage of 0.2, 0.4, 0.5, 0.7, 0.8, 0.9 or any two value ranges.
Further, the mass percent usage of ceramide NP is 0.4, 0.8, 1.0, 1.5, 1.8, 1.9 or any two ranges of values.
Further, the mass percent amount of stearyl glycyrrhetinate is 0.2, 0.4, 0.5, 0.7, 0.8, 0.9, or any two ranges of values.
Further, the phosphatidylcholine is used in a mass percent amount of 0.5, 1, 2, 3, 4, 5, 6, 7, 8, 9 or any two ranges of values.
Further, the cholesterol is used in a mass percent amount of 0.2, 0.5, 0.8, 1.2, 2, 3, 4 or any two ranges of values.
Further, the mass percent of phytosphingosine is used in an amount of 0.2, 0.5, 0.8, 1.2, 2, 3, 4 or any two ranges of values.
Further, the tocopherol is used in a mass percent amount of 0.2, 0.4, 0.5, 0.7, 0.8, 0.9, or any two ranges of values.
Further, the glycerol is used in a mass percent amount of 22, 25, 30, 35, 40, 45, 50, 55, 58 or any two ranges of values.
Further, the water is used in a mass percent amount of 14.5, 15, 16, 18, 20, 25, 30, 35, 40, 45, 50, 55, 58 or any two ranges of values.
The invention provides a preparation method of liposome for wrapping a soothing and repairing component by using a micro-jet homogenizer, which is characterized by comprising the following steps of: the method comprises the following steps:
(1) Weighing centella asiatica extract complex, dendrobium nobile extract, ceramide NP, stearyl glycyrrhetinate, phosphatidylcholine, cholesterol, phytosphingosine, tocopherol, glycerol and water;
pretreatment of raw materials: dissolving ceramide NP, herba Centellae extract complex, stearyl glycyrrhetinate, phosphatidylcholine, cholesterol, phytosphingosine and tocopherol in organic solvent, ultrasonically dissolving for 2-120min under the conditions of ultrasonic frequency of 20-100KHz and power of 80-320W, and stirring at 20-70deg.C and stirring speed of 20-500 r/min for 0.2-5 hr to obtain oil phase;
(2) Mixing glycerol, herba Dendrobii extract and water at 20-70deg.C under stirring at 20-500 rpm for 0.2-5 hr to obtain water phase;
(3) Pouring the water phase into the oil phase, stirring for 0.5-6 hours at the temperature of 30-75 ℃ and the stirring speed of 50-800 rpm, and mixing to obtain a pre-emulsion;
(4) Homogenizing the pre-emulsion by using a micro-jet homogenizer under the pressure of 20-300MPa for 2-120min to obtain the liposome.
In another aspect, the present invention provides a liposome prepared by the above preparation method.
In another aspect, the invention provides the use of said liposomes in cosmetics in the form of an aqueous, emulsion, cream, ointment, essence or mask.
The beneficial effects are that:
the ceramide NP in the liposome prepared by the process is uniformly dispersed and can be stably present in the liposome; the preparation method of the liposome does not contain solubilizer, preservative and permeation aid, and the obtained liposome is bubble-free and has the effects of nano particle size, strong efficacy, good absorption, low irritation and good stability; the preparation method enables the effects of various soothing components, moisturizing, repairing and maintaining active components such as skin to be better exerted, and endows the liposome with excellent effects of soothing skin, moisturizing, repairing and maintaining skin.
The liposome obtained by the preparation method of the liposome for wrapping the soothing and repairing components by using the micro-jet homogenizer has excellent soothing effect, can obviously reduce the effect of skin haematochrome and red area, reduces the ratio of haematochrome to 12.86%, and reduces the ratio of red area to 18.35%.
The liposome obtained by the preparation method of the liposome wrapping the soothing and repairing components by using the micro-jet homogenizer has excellent moisturizing and repairing skin effects, can obviously increase the skin moisture content and reduce the skin percutaneous moisture loss, achieves 35.6% on the effect of increasing the skin moisture content ratio, and achieves 28.6% on the effect of reducing the skin percutaneous moisture loss ratio.
The invention obtains uniform ceramide NP-phosphatidylcholine-centella asiatica extract compound-stearyl glycyrrhetinate-tocopherol oil phase by the raw material pretreatment process. The pretreatment operation ensures that the ceramide NP-phosphatidylcholine-centella asiatica extract complex-stearyl glycyrrhetinate-tocopherol is fully micronized and homogenized in an organic solvent, thereby effectively reducing the crystallinity of the ceramide NP and improving the compatibility of the ceramide NP and liposome components.
The invention can obviously increase the exertion of active ingredients of liposome by using a micro-jet homogenization process, and endow the product with excellent relieving effect. The nano-carrier is formed by the process to encapsulate the functional active substances to form tiny particles, so that ceramide exists stably in a lipid system, better encapsulation effect is given to the active ingredients, the active substances are stably conveyed, the effect of reducing skin red pigment and red area by the liposome is increased, and meanwhile, excellent moisturizing, repairing and skin maintaining effects are given to the liposome.
The process of the invention selects proper oil phase composition and water phase composition, and then the oil phase and water phase are mixed for pre-emulsification, so that the stability of the effective components of the liposome can be improved, and the effects of relieving, moisturizing, repairing and maintaining the skin can be exerted.
The invention uses ceramide NP, centella asiatica extract complex and stearyl glycyrrhetinate to endow the liposome with excellent comfort and moisture-preserving effects. In the dosage range of the invention and the liposome system, the compounding of ceramide NP, centella asiatica extract complex and stearyl glycyrrhetinate can generate a mutual forward promotion relationship in increasing the effects of relieving and moisturizing.
Detailed Description
The advantages and various effects of the present invention will be more clearly apparent from the following detailed description and examples. It will be understood by those skilled in the art that these specific embodiments and examples are intended to illustrate the invention, not to limit the invention.
Throughout the specification, unless specifically indicated otherwise, the terms used herein should be understood as meaning as commonly used in the art. Accordingly, unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. In case of conflict, the present specification will control.
Unless otherwise specifically indicated, the various raw materials, reagents, instruments, equipment and the like used in the present invention are commercially available or may be prepared by existing methods.
The invention relates to a test group, wherein the hydroxy asiaticoside, asiaticoside and asiatic centella leaf extract are from Qixian Hua Du essence and spice (Guangzhou) limited company; the dendrobium nobile extract is derived from the plant extract biotechnology limited company in the Qingxi county; ceramide NP is derived from Chongqing Zhi He biomedical Co.
Test group 1:
a preparation method of liposome for wrapping the soothing and repairing components by using a micro-jet homogenizer comprises the following steps:
(1) Weighing the following raw materials in percentage by mass: 0.8% centella asiatica extract complex, 0.6% dendrobium nobile extract, 0.7% ceramide NP, 0.82% stearyl glycyrrhetinate, 8.5% phosphatidylcholine, 3.8% cholesterol, 1.2% phytosphingosine, 0.4% tocopherol, 15% water and the balance glycerol; wherein, the centella extract compound comprises the following components in mass ratio of 50:15:35 madecassoside, a mixture of asiaticoside and asiatic centella leaf extract;
pretreatment of raw materials: dissolving ceramide NP, herba Centellae extract complex, stearyl glycyrrhetinate, phosphatidylcholine, cholesterol, phytosphingosine, and tocopherol in organic solvent ethanol; ultrasonic dissolving for 20 minutes under the conditions of ultrasonic frequency of 40KHz and power of 180W, stirring for 0.5 hour at the temperature of 45 ℃ and the stirring rotation speed of 400 r/min, mixing, transferring to a rotary evaporator, and removing organic solvent ethanol to obtain ceramide NP-phosphatidylcholine-centella asiatica extract complex-stearyl glycyrrhetinate-tocopherol oil phase;
wherein, the mass ratio of ceramide NP, centella asiatica extract complex, stearyl glycyrrhetinate, phosphatidylcholine, cholesterol, phytosphingosine, tocopherols and organic solvent ethanol is 1:30;
(2) Mixing herba Dendrobii extract, water and glycerol at 45deg.C under stirring at 100 rpm for 0.5 hr to obtain water phase;
(3) Pouring the water phase into the oil phase, and mixing for 2 hours at the temperature of 50 ℃ and the stirring rotation speed of 200 revolutions per minute to obtain a pre-emulsion;
(4) Homogenizing the pre-emulsion for 10min under 150MPa by using an MF7250IP-EH production type high-pressure micro-jet homogenizer of Shanghai Miao Biotechnology Co.
Test group 2:
a preparation method of liposome for wrapping the soothing and repairing components by using a micro-jet homogenizer comprises the following steps:
(1) Weighing the following raw materials in percentage by mass: 0.78% centella asiatica extract complex, 0.55% dendrobium nobile extract, 0.73% ceramide NP, 0.85% stearyl glycyrrhetinate, 7.6% phosphatidylcholine, 4.0% cholesterol, 1.2% phytosphingosine, 0.4% tocopherol, 15.3% water and the balance glycerol; wherein, the centella extract compound comprises the following components in mass ratio of 50:15:35 madecassoside, a mixture of asiaticoside and asiatic centella leaf extract;
pretreatment of raw materials: dissolving ceramide NP, herba Centellae extract complex, stearyl glycyrrhetinate, phosphatidylcholine, cholesterol, phytosphingosine, and tocopherol in organic solvent ethanol; ultrasonic dissolving for 18 min under the conditions of ultrasonic frequency of 45KHz and power of 200W, stirring for 1 hour at the temperature of 50 ℃ and the stirring rotation speed of 300 r/min, mixing, transferring to a rotary evaporator, and removing organic solvent ethanol to obtain ceramide NP-phosphatidylcholine-centella asiatica extract complex-stearyl glycyrrhetinate-tocopherol oil phase;
wherein, the mass ratio of ceramide NP, centella asiatica extract complex, stearyl glycyrrhetinate, phosphatidylcholine, cholesterol, phytosphingosine, tocopherols and organic solvent ethanol is 1:30;
(2) Mixing herba Dendrobii extract, water and glycerol at 50deg.C under stirring at 100 rpm for 0.2 hr to obtain water phase;
(3) Pouring the water phase into the oil phase, and mixing for 1.8 hours under the conditions that the temperature is 55 ℃ and the stirring speed is 220 rpm, so as to obtain a pre-emulsion;
(4) Homogenizing the pre-emulsion for 8min under a homogenizing pressure of 500MPa by using an MF7250IP-EH production type high-pressure micro-jet homogenizer of Shanghai Miao Biotechnology Co.
Test group 3:
a method for preparing liposome for wrapping and soothing components, comprising the following steps:
(1) Weighing the following raw materials in percentage by mass: 0.8% centella asiatica extract complex, 0.6% dendrobium nobile extract, 0.7% ceramide NP, 0.82% stearyl glycyrrhetinate, 8.5% phosphatidylcholine, 3.8% cholesterol, 1.2% phytosphingosine, 0.4% tocopherol, 15% water and the balance glycerol; wherein, the centella extract compound comprises the following components in mass ratio of 50:15:35 madecassoside, a mixture of asiaticoside and asiatic centella leaf extract;
pretreatment of raw materials: dissolving ceramide NP, herba Centellae extract complex, stearyl glycyrrhetinate, phosphatidylcholine, cholesterol, phytosphingosine, and tocopherol in organic solvent ethanol; ultrasonic dissolving for 20 minutes under the conditions of ultrasonic frequency of 40KHz and power of 180W, stirring for 0.5 hour at the temperature of 45 ℃ and the stirring rotation speed of 400 r/min, mixing, transferring to a rotary evaporator, and removing organic solvent ethanol to obtain ceramide NP-phosphatidylcholine-centella asiatica extract complex-stearyl glycyrrhetinate-tocopherol oil phase;
wherein, the mass ratio of ceramide NP, centella asiatica extract complex, stearyl glycyrrhetinate, phosphatidylcholine, cholesterol, phytosphingosine, tocopherols and organic solvent ethanol is 1:30;
(2) Mixing herba Dendrobii extract, water and glycerol under stirring at 55deg.C and stirring speed of 100 rpm for 0.2 hr to obtain water phase;
(3) Pouring the water phase into the oil phase, and mixing for 2 hours at the temperature of 50 ℃ and the stirring rotation speed of 200 revolutions per minute to obtain a pre-emulsion;
(4) Stirring the pre-emulsion for 0.5 hour at the rotation speed of 5000 rpm to obtain the liposome.
Test group 4:
a preparation method of liposome for wrapping the soothing and repairing components by using a micro-jet homogenizer comprises the following steps:
(1) Weighing the following raw materials in percentage by mass: 0.8% centella asiatica extract complex, 0.6% dendrobium nobile extract, 0.7% ceramide NP, 0.82% stearyl glycyrrhetinate, 8.5% phosphatidylcholine, 3.8% cholesterol, 1.2% phytosphingosine, 0.4% tocopherol, 15% water and the balance glycerol; wherein, the centella extract compound comprises the following components in mass ratio of 50:15:35 madecassoside, a mixture of asiaticoside and asiatic centella leaf extract;
pretreatment of raw materials: dissolving ceramide NP, herba Centellae extract complex, stearyl glycyrrhetinate, phosphatidylcholine, cholesterol, phytosphingosine, tocopherol, herba Dendrobii extract, and glycerol in organic solvent ethanol; ultrasonic dissolving for 20 minutes under the conditions of ultrasonic frequency of 40KHz and power of 180W, stirring for 0.5 hour at the temperature of 45 ℃ and the stirring rotation speed of 400 r/min, mixing, transferring to a rotary evaporator, and removing organic solvent ethanol to obtain an oil phase of ceramide NP-phosphatidylcholine-centella asiatica extract complex-stearyl glycyrrhetinate-tocopherol-dendrobium nobile extract-glycerin;
wherein, the mass ratio of the total mass of ceramide NP, centella asiatica extract complex, stearyl glycyrrhetinate, phosphatidylcholine, cholesterol, phytosphingosine, tocopherol, dendrobium nobile extract and glycerin to the organic solvent ethanol is 1:30;
(2) Stirring and mixing water for 0.2 hour under the conditions that the temperature is 55 ℃ and the stirring rotation speed is 100 revolutions per minute to obtain a water phase;
(3) Pouring the water phase into the oil phase, and mixing for 2 hours at the temperature of 50 ℃ and the stirring rotation speed of 200 revolutions per minute to obtain a pre-emulsion;
(4) Homogenizing the pre-emulsion for 10min under 150MPa by using an MF7250IP-EH production type high-pressure micro-jet homogenizer of Shanghai Miao Biotechnology Co.
Test group 5:
a preparation method of liposome for wrapping the soothing and repairing components by using a micro-jet homogenizer comprises the following steps:
(1) Weighing the following raw materials in percentage by mass: 0.8% centella asiatica extract complex, 0.6% dendrobium nobile extract, 0.7% ceramide NP, 0.82% stearyl glycyrrhetinate, 8.5% phosphatidylcholine, 3.8% cholesterol, 1.2% phytosphingosine, 0.4% tocopherol, 15% water and the balance glycerol; wherein, the centella extract compound comprises the following components in mass ratio of 50:15:35 madecassoside, a mixture of asiaticoside and asiatic centella leaf extract;
pretreatment of raw materials: dissolving herba Centellae extract complex, stearyl glycyrrhetinate, phosphatidylcholine, cholesterol, phytosphingosine and tocopherol in organic solvent ethanol; ultrasonic dissolving for 20min under the conditions of ultrasonic frequency of 40KHz and power of 180W, stirring for 0.5 hour at 45 ℃ and stirring rotation speed of 400 r/min, mixing, transferring to a rotary evaporator, and removing organic solvent to obtain phosphatidylcholine-centella asiatica extract complex-stearyl glycyrrhetinate-tocopherol oil phase;
wherein the mass ratio of centella asiatica extract complex, stearyl glycyrrhetinate, phosphatidylcholine, cholesterol, phytosphingosine, total tocopheryl soluble mass and organic solvent ethanol is 1:30;
(2) Mixing ceramide NP, herba Dendrobii extract, water and glycerol under stirring at 55deg.C and stirring speed of 100 rpm for 0.1 hr to obtain water phase;
(3) Pouring the water phase into the oil phase, and mixing for 2 hours at the temperature of 50 ℃ and the stirring rotation speed of 200 revolutions per minute to obtain a pre-emulsion;
(4) Homogenizing the pre-emulsion for 10min under 150MPa by using an MF7250IP-EH production type high-pressure micro-jet homogenizer of Shanghai Miao Biotechnology Co.
Test group 6:
the difference from test group 1 was only that the centella asiatica extract complex was not contained, the amount of ceramide NP was 1.5%, and the other was the same as in example 1.
Test group 7:
the difference from test group 1 was only that no ceramide NP was contained, and the amount of centella asiatica extract complex was changed to 1.5%, and the other was the same as in example 1.
Test group 8:
the difference from test group 1 was only that stearyl glycyrrhetinate was not contained, the amount of centella asiatica extract complex was changed to 1.62%, and the other was the same as in example 1.
Performance testing
The liposomes of test groups 1-8 above were subjected to performance testing.
1. Test of soothing Effect
140 subjects between 35 and 50 years of age were selected for randomized classification into 8 groups of 20 persons each, 10 men and women each. Each group of subjects used 1.5g of liposomes from test group 1-8 at the left face daily, in the morning and evening, for 4 weeks. Skin tests were performed at weeks 0 and 4 using the seventh generation of VISIA and MPA580 to test for red pigment and red area index, and then the average value of each group was calculated, and the results obtained are shown in table 1.
TABLE 1
From the test results in table 1, it is known that the liposome obtained by the preparation method of the liposome for wrapping the soothing component by using the micro-jet homogenizer has excellent soothing effect, can obviously reduce the effect of skin haematochrome and red region, reduces the ratio of haematochrome to 12.86%, and reduces the ratio of red region to 18.35%.
As can be seen from the comparison of the test group 1 and the test group 3, the present invention can significantly increase the exertion of the active ingredients of the liposome by using the micro-jet homogenization process, and gives the product an excellent soothing effect. The technology forms micro-nano carriers to encapsulate the functional active substances to form tiny particles, so that ceramide stably exists in a lipid system, better dispersing effect is given to the active ingredients, the active substances are stably conveyed, and the effect of reducing skin red pigment and red area of the liposome is increased.
As can be seen from a comparison of test group 1 and test groups 4-5, the process of the present invention selects suitable oil phase and water phase compositions, and the process of pre-emulsifying the oil phase and water phase mixture can increase the stability of the liposome effective components and exert the soothing effect.
As can be seen from the comparison of test group 1 with test groups 6-8, the use of ceramide NP, centella asiatica extract complex and stearyl glycyrrhetinate in the stock dosage system of the present invention imparts excellent soothing effects to the liposomes. When the amount of ceramide NP or centella asiatica extract complex in test group 6-7 is the same as the total amount of ceramide NP and centella asiatica extract complex in test group 1, the liposomes in test group 1 have more excellent effect of reducing skin redness and red area, thereby demonstrating that the ceramide NP and centella asiatica extract complex in the system of the present invention have a synergistic relationship in providing soothing skin effect, and the combination of both has a synergistic effect in increasing soothing effect. In comparison with test group 1, it is clear that the effect of the liposome is inferior to that of test group 1, since stearyl glycyrrhetinate is omitted and an equivalent amount of centella asiatica extract complex is added, the effect of the stearyl glycyrrhetinate in the liposome system of the present invention can be further promoted.
2. Skin moisturizing and repairing effect test
The skin surface inside the forearm of the test subjects was tested for changes in moisture content and transdermal moisture loss, and the moisturizing and skin-repairing effects of the liposomes of test groups 1-8 were characterized.
Several subjects with 35-50 years old and dry skin inside the arms were selected, randomly divided into 8 groups of 20 subjects each, 10 subjects each. Group 1-8 subjects used the liposomes of test groups 1-8 above at 1.8mg/cm 2 Is applied in a single application and is uniformly applied to the test area of the skin surface inside the forearm of the subject, and the skin cuticle moisture value and skin percutaneous moisture loss are detected by using MPA 580. Test subjects were tested for values before and after 10 hours of use of the liposomes of each group; the experimental conditions are as follows: temperature (25.+ -. 0.5) DEG C, relative humidity (55.+ -. 5)%. Then, the rate of change Q of the moisture content of the skin stratum corneum and the rate of change of the water loss of skin through skin are calculated after 10 hours of useK and the results are shown in Table 2.
TABLE 2
From the test results in table 2, it is clear that the liposome obtained by the preparation method of the liposome for wrapping the soothing and repairing component by using the micro-jet homogenizer has excellent moisturizing and repairing skin effects, can remarkably increase the skin moisture content and reduce the skin percutaneous moisture loss, achieves 35.6% on the effect of increasing the skin moisture content ratio, and achieves 28.6% on the effect of reducing the skin percutaneous moisture loss ratio.
As can be seen from the comparison of the test group 1 and the test group 3, the invention can obviously increase the exertion of the active ingredients of the liposome by using the micro-jet homogenization process, and endow the product with excellent moisturizing and skin-repairing effects. The technology forms the micro-nano carrier to wrap the functional active substances to form tiny particles, so that the ceramide stably exists in a lipid system, better dispersing effect is given to the active ingredients, the active substances are stably conveyed, and the moisturizing and skin repairing effects of the liposome are improved.
As can be seen from the comparison of the test group 1 and the test groups 4-5, the process provided by the invention selects the proper oil phase and water phase to form, and the process of mixing the oil phase and the water phase for pre-emulsification can increase the stability of the liposome functional components and exert the moisturizing and skin-repairing effects.
As can be seen from the comparison of test group 1 and test groups 6-8, the use of ceramide NP, centella asiatica extract complex and stearyl glycyrrhetinate in the raw material dosage system of the present invention can impart excellent moisturizing effect to the liposome; the dosage range of the invention and the liposome system have a mutual promotion relationship in the aspect of increasing the skin moisturizing and repairing effects by compounding the components.
It will be apparent to those skilled in the art that various modifications and variations can be made to the present invention without departing from the spirit or scope of the invention. Thus, it is intended that the present invention also include such modifications and alterations insofar as they come within the scope of the appended claims or the equivalents thereof.

Claims (10)

1. A preparation method for preparing liposome for wrapping a soothing and repairing component by using a micro-jet homogenizer is characterized by comprising the following steps of: the method comprises the following steps:
(1) Weighing raw materials: centella asiatica extract complex, dendrobium nobile extract, ceramide NP, stearyl glycyrrhetinate, phosphatidylcholine, cholesterol, phytosphingosine, tocopherol, glycerin, and water; wherein the centella extract complex is a mixture of madecassoside and asiaticoside and centella leaf extract;
pretreatment of raw materials: dissolving ceramide NP, phosphatidylcholine, centella asiatica extract complex, stearyl glycyrrhetinate, cholesterol, phytosphingosine and tocopherol in an organic solvent, ultrasonically dissolving, uniformly stirring, and transferring to a rotary evaporator to remove the organic solvent to obtain a ceramide NP-phosphatidylcholine-centella asiatica extract complex-stearyl glycyrrhetinate-tocopherol oil phase;
(2) Mixing glycerol, herba Dendrobii extract and water to obtain water phase;
(3) Pouring the water phase into the oil phase for mixing, and uniformly stirring to obtain a pre-emulsion;
(4) Homogenizing the pre-emulsion by using a micro-jet homogenizer to obtain the liposome.
2. The method of preparing a liposome according to claim 1, wherein: the micro-jet homogenizer is a micifuga micro-jet homogenizer.
3. The method of preparing a liposome according to claim 1, wherein: the homogenizing pressure of the micro-jet machine is 20-300MPa.
4. The method of preparing a liposome according to claim 1, wherein: the homogenizing pressure of the micro-jet machine is 30-250MPa.
5. The method of preparing a liposome according to claim 1, wherein: the homogenizing pressure of the micro-jet machine is 50-250MPa.
6. The method of preparing a liposome according to claim 1, wherein: the homogenizing time of the micro-jet machine is 2-120min.
7. The method of preparing a liposome according to claim 1, wherein: the homogenizing time of the micro-jet machine is 3-30min.
8. The method of preparing a liposome according to claim 1, wherein: the raw materials comprise the following components: 0.1-1% centella asiatica extract complex, 0.1-1% dendrobium nobile extract, 0.1-2% ceramide NP, 0.1-1% stearyl glycyrrhetinate, 0.1-10% phosphatidylcholine, 0.1-5% cholesterol, 0.1-5% phytosphingosine, 0.1-1% tocopherol, 20-60% glycerin and 14-75% water; wherein, the centella extract compound comprises the following components in mass ratio of 50:15:35 madecassoside, asiaticoside and centella asiatica leaf extract.
9. A liposome prepared by the method of any one of claims 1-8.
10. Use of the liposomes according to claim 9 in cosmetics in the form of aqueous solutions, emulsions, creams, ointments, essences or masks.
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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106691889A (en) * 2015-11-12 2017-05-24 武汉百思凯瑞纳米科技有限公司 High skin retention ceramide nano composition, and preparation method and applications thereof
KR20180032479A (en) * 2016-09-22 2018-03-30 프롬바이오 주식회사 Nano Liposome Composition Comprising Peptide for Easy Penetrating into Skin
CN113116768A (en) * 2020-01-10 2021-07-16 广州市科能化妆品科研有限公司 Water dew and collagenase inhibitor and preparation method thereof
CN113662879A (en) * 2021-08-31 2021-11-19 珀莱雅化妆品股份有限公司 Salt-tolerant ceramide liposome with skin repairing effect and preparation method thereof
CN115429713A (en) * 2022-10-12 2022-12-06 广州菲科日用化工有限公司 Moisturizing, repairing and anti-aging composition containing ceramide and preparation method thereof

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106691889A (en) * 2015-11-12 2017-05-24 武汉百思凯瑞纳米科技有限公司 High skin retention ceramide nano composition, and preparation method and applications thereof
KR20180032479A (en) * 2016-09-22 2018-03-30 프롬바이오 주식회사 Nano Liposome Composition Comprising Peptide for Easy Penetrating into Skin
CN113116768A (en) * 2020-01-10 2021-07-16 广州市科能化妆品科研有限公司 Water dew and collagenase inhibitor and preparation method thereof
CN113662879A (en) * 2021-08-31 2021-11-19 珀莱雅化妆品股份有限公司 Salt-tolerant ceramide liposome with skin repairing effect and preparation method thereof
CN115429713A (en) * 2022-10-12 2022-12-06 广州菲科日用化工有限公司 Moisturizing, repairing and anti-aging composition containing ceramide and preparation method thereof

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