CN113546009A - Water-in-oil type rutin microemulsion and preparation method thereof - Google Patents

Water-in-oil type rutin microemulsion and preparation method thereof Download PDF

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Publication number
CN113546009A
CN113546009A CN202110869380.2A CN202110869380A CN113546009A CN 113546009 A CN113546009 A CN 113546009A CN 202110869380 A CN202110869380 A CN 202110869380A CN 113546009 A CN113546009 A CN 113546009A
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Prior art keywords
oil
rutin
phase
microemulsion
water
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宋晓秋
杜嘉蕊
叶琳
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Shanghai Institute of Technology
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Shanghai Institute of Technology
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    • AHUMAN NECESSITIES
    • 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
    • A61K8/92Oils, fats or waxes; Derivatives thereof, e.g. hydrogenation products thereof
    • A61K8/922Oils, fats or waxes; Derivatives thereof, e.g. hydrogenation products thereof of vegetable origin
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/02Cosmetics or similar toiletry preparations characterised by special physical form
    • A61K8/04Dispersions; Emulsions
    • A61K8/06Emulsions
    • A61K8/068Microemulsions
    • AHUMAN NECESSITIES
    • 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
    • A61K8/33Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing oxygen
    • A61K8/34Alcohols
    • A61K8/345Alcohols containing more than one hydroxy group
    • AHUMAN NECESSITIES
    • 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
    • A61K8/60Sugars; Derivatives thereof
    • A61K8/602Glycosides, e.g. rutin
    • AHUMAN NECESSITIES
    • 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
    • A61K8/72Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds
    • A61K8/84Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds obtained by reactions otherwise than those involving only carbon-carbon unsaturated bonds
    • A61K8/86Polyethers
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61QSPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q17/00Barrier preparations; Preparations brought into direct contact with the skin for affording protection against external influences, e.g. sunlight, X-rays or other harmful rays, corrosive materials, bacteria or insect stings
    • A61Q17/04Topical preparations for affording protection against sunlight or other radiation; Topical sun tanning preparations
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61QSPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q19/00Preparations for care of the skin
    • A61Q19/08Anti-ageing preparations

Abstract

The invention discloses a water-in-oil type rutin microemulsion and a preparation method thereof. The rutin microemulsion comprises an emulsifier, a solvent, rutin and an oil phase. The preparation method comprises the steps of oscillating and mixing the oil phase and the emulsifier uniformly at room temperature to obtain a phase A, dissolving rutin in a solvent to obtain a phase B, adding the phase B into the phase A under the stirring condition, and oscillating to obtain the water-in-oil rutin microemulsion. The microemulsion prepared by the invention solves the problem that rutin can not be dissolved in grease, protects the rutin from being oxidized and losing efficacy by using the grease, can keep good stability at 5-40 ℃, has the characteristics of clarity and transparency, enables the rutin to better absorb ultraviolet rays, and has wide application value.

Description

Water-in-oil type rutin microemulsion and preparation method thereof
Technical Field
The invention relates to a water-in-oil type rutin microemulsion and a preparation method thereof, belonging to the technical field of cosmetics.
Background
Rutin and vitamin P are in form of light yellow or light green needle crystals or crystalline powder, exist in herba Pelargonii Graveolentis, tobacco leaf, fructus Jujubae, fructus Pruni, pericarpium Citri Junoris, fructus Lycopersici Esculenti, and flos Fagopyri Esculenti, and can be used as natural sunscreen agent for absorbing ultraviolet to resist skin photoaging; rutin also has effects of scavenging active oxygen free radicals generated by cells, and achieving antioxidation effect. Is mainly used for preparing sunscreen and anti-aging cosmetics.
Rutin is poorly soluble in water and oil phases, fails to meet practical cosmetic application requirements, and is unstable due to temperature and pH effects.
Disclosure of Invention
The technical problem to be solved by the invention is as follows: because rutin is difficult to dissolve in water and oil phase, the application requirements of practical cosmetics cannot be met, and the rutin is unstable under the influence of temperature and pH.
In order to solve the technical problem, the invention provides a water-in-oil type rutin microemulsion, which comprises an emulsifier, a solvent, rutin and an oil phase; the emulsifier is at least one of polyglycerol ricinoleate, tween-80, span-80, glyceryl oleate and castor oil polyoxyethylene ether-20, the oil phase is at least one of lavender essential oil, refined coconut oil, olive oil, soybean oil, jojoba oil and castor oil, and the solvent is at least one of absolute ethyl alcohol, 1, 2-propylene glycol, 1, 3-butanediol, 1, 2-pentanediol, polyethylene glycol-400 and sorbitol.
The invention also provides a preparation method of the water-in-oil rutin microemulsion, which comprises the following steps:
step 1: mixing the oil phase and the emulsifier in proportion at room temperature, uniformly stirring, transferring to a container, and placing on a constant temperature oscillator for continuous shaking to obtain a phase A;
step 2: weighing rutin powder at room temperature, dissolving in solvent, heating, stirring, and dissolving until clear transparent solution is obtained to obtain phase B;
and step 3: and adding the phase B into the phase A, and placing the phase A on a constant temperature oscillator to continuously shake for 12-24 hours at the temperature of 20-30 ℃ to obtain the water-in-oil rutin microemulsion.
Preferably, the mass ratio of the oil phase to the emulsifier in the step 1 is 3-8: 2 to 7.
Preferably, the conditions of the continuous shaking on the constant temperature oscillator in the step 1 are as follows: the temperature is 20-30 ℃, and the time is 12-24 h.
Preferably, the mass ratio of the rutin powder to the solvent in the step 2 is 0.2-0.6: 8 to 16.
Preferably, the heating and stirring temperature in the step 2 is 70-90 ℃.
Preferably, the mass ratio of the phase A to the phase B in the step 3 is 1: 0.01 to 0.1.
Preferably, the conditions of the continuous shaking on the constant temperature oscillator in the step 3 are as follows: the temperature is 20-30 ℃, and the time is 12-24 h.
Compared with the prior art, the invention has the beneficial effects that:
1. the water-in-oil rutin microemulsion is prepared by dissolving rutin in a solvent, so that the rutin is applied to an oil phase, the technical problem that the rutin is difficult to dissolve in water and the oil phase and is unstable due to the influence of temperature and pH is solved, and the application requirements of practical cosmetics can be met;
2. the water-in-oil rutin microemulsion disclosed by the invention uses grease to protect rutin from being oxidized and losing efficacy, can keep good stability at 5-40 ℃, has the characteristics of clarity and transparency, enables rutin to better absorb ultraviolet rays, and has a wide application value.
Detailed Description
In order to make the invention more comprehensible, preferred embodiments are described in detail below.
In the following examples, the raw materials used were commercially available products, and the specifications and manufacturer information of the raw materials or reagents used are shown in table 1:
TABLE 1 reagent information
Figure BDA0003188410900000021
Figure BDA0003188410900000031
In the following examples, some of the equipment manufacturers and models used are shown in Table 2:
TABLE 2 Instrument information
Instrumentation and equipment Model number Manufacturer of the product
Electronic balance PL403 Mettler-Tollido instruments Ltd
Digital display constant temperature water bath HH-2 Shanghai Lichen Bangxi Instrument science and technology Co Ltd
Water bath constant temperature oscillator SHZ-B Shanghai Boxun Medical Biological Instrument Corp.
Manual liquid transfer device 100μL Mettler-Tollido instruments Ltd
Example 1
A water-in-oil type rutin microemulsion is prepared by using castor oil polyoxyethylene ether-20 and span-80 as emulsifier, olive oil as oil phase, and polyethylene glycol-400 as solvent.
The preparation method of the water-in-oil rutin microemulsion specifically comprises the following steps:
(1) mixing the oil phase and the emulsifier according to a certain proportion at room temperature, uniformly stirring, transferring to a container, placing on a constant temperature oscillator, and continuously shaking for 12h at the temperature of 25 ℃ to obtain a phase A;
the dosage of the oil phase and the emulsifier is as follows according to the mass ratio: the proportion of the emulsifier is 4: 6;
the emulsifier is compounded by castor oil polyoxyethylene ether-20 and span-80 in a ratio of 1: 4;
(2) weighing rutin powder at room temperature, dissolving in solvent, placing beaker in 80 deg.C water bath, heating, stirring, and dissolving until clear transparent solution is obtained to obtain phase B;
the dosage of the rutin powder and the solvent is as follows: calculating the mass ratio of the solvent to be 0.4: 8;
(3) adding the phase B into the phase A, placing the phase A on a constant temperature oscillator, and continuously shaking for 12-24 h at the temperature of 20-30 ℃ to obtain a water-in-oil rutin microemulsion;
the dosage of the phase A and the phase B is as follows according to the mass ratio of the phase A: phase B is 1: a ratio calculation of 0.045;
the solubility of rutin in oil and fat in the obtained water-in-oil rutin microemulsion is improved by 2.25 times (the solubility of rutin in oil and fat at room temperature of 25 ℃ is below 0.01g/100 g) at most, and the water-in-oil rutin microemulsion is clear and transparent.
Example 2
A water-in-oil type rutin microemulsion is prepared by using glyceryl oleate as emulsifier, oleum Olivarum as oil phase, and polyethylene glycol-400 as solvent;
the preparation method of the water-in-oil rutin microemulsion specifically comprises the following steps:
(1) mixing the oil phase and the emulsifier according to a certain proportion at room temperature, uniformly stirring, transferring to a container, placing on a constant temperature oscillator, and continuously shaking for 12h at the temperature of 25 ℃ to obtain a phase A;
the dosage of the oil phase and the emulsifier is as follows: the mass ratio of the emulsifier is calculated as 1: 1;
(2) weighing rutin powder at room temperature, dissolving in solvent, placing beaker in 80 deg.C water bath, heating, stirring, and dissolving until clear transparent solution is obtained to obtain phase B;
the dosage of the rutin powder and the solvent is as follows: calculating the mass ratio of the solvent to be 0.4: 8;
(3) adding the phase B into the phase A, placing the phase A on a constant temperature oscillator, and continuously shaking for 12-24 h at the temperature of 20-30 ℃ to obtain a water-in-oil rutin microemulsion;
the dosage of the phase A and the phase B is as follows according to the mass ratio of the phase A: calculating the proportion of the phase B to be 1: 0.075;
the solubility of rutin in oil and fat in the obtained water-in-oil rutin microemulsion is improved by 3.75 times (the solubility of rutin in oil and fat at room temperature of 25 ℃ is below 0.01g/100 g) to the maximum, and the water-in-oil rutin microemulsion is clear and transparent.
Heat resistance and cold resistance test:
the water-in-oil rutin microemulsion of example 2 was placed in an environment of 5 deg.C, 25 deg.C, 40 deg.C for 6h, 12h, and 24h, respectively, and the microemulsion state was observed, with the results shown in Table 3.
TABLE 3 Heat and Cold resistance test results
Test number Test temperature/. degree.C Test time/h Microemulsion state
1 5 6 Clear and transparent
2 5 12 Clear and transparent
3 5 24 Clear and transparent
4 25 6 Clear and transparent
5 25 12 Clear and transparent
6 25 24 Clear and transparent
7 40 6 Clear and transparent
8 40 12 Clear and transparent
9 40 24 Clear and transparent
The results in table 1 show that the water-in-oil rutin microemulsion of the present invention can maintain good stability at 5-40 ℃, has good heat resistance and cold resistance, and can be widely applied to cosmetics.
The above-described embodiments are only preferred embodiments of the present invention, and are not intended to limit the present invention in any way and substantially, it should be noted that those skilled in the art may make several modifications and additions without departing from the scope of the present invention, which should also be construed as a protection scope of the present invention.

Claims (8)

1. A water-in-oil type rutin microemulsion is characterized by comprising an emulsifier, a solvent, rutin and an oil phase; the emulsifier is at least one of polyglycerol ricinoleate, tween-80, span-80, glyceryl oleate and castor oil polyoxyethylene ether-20, the oil phase is at least one of lavender essential oil, refined coconut oil, olive oil, soybean oil, jojoba oil and castor oil, and the solvent is at least one of absolute ethyl alcohol, 1, 2-propylene glycol, 1, 3-butanediol, 1, 2-pentanediol, polyethylene glycol-400 and sorbitol.
2. The preparation method of water-in-oil rutin microemulsion as claimed in claim 1, which comprises the following steps:
step 1: mixing the oil phase and the emulsifier in proportion at room temperature, uniformly stirring, transferring to a container, and placing on a constant temperature oscillator for continuous shaking to obtain a phase A;
step 2: weighing rutin powder at room temperature, dissolving in solvent, heating, stirring, and dissolving until clear transparent solution is obtained to obtain phase B;
and step 3: and adding the phase B into the phase A, and placing the phase A on a constant temperature oscillator to continuously shake for 12-24 hours at the temperature of 20-30 ℃ to obtain the water-in-oil rutin microemulsion.
3. The preparation method of the water-in-oil rutin microemulsion as claimed in claim 2, wherein the mass ratio of the oil phase and the emulsifier in the step 1 is 3-8: 2 to 7.
4. The process for preparing a water-in-oil rutin microemulsion as claimed in claim 2, wherein the conditions of the continuous shaking on the constant temperature oscillator in step 1 are as follows: the temperature is 20-30 ℃, and the time is 12-24 h.
5. The preparation method of water-in-oil rutin microemulsion as claimed in claim 2, wherein the weight ratio of rutin powder and solvent in step 2 is 0.2-0.6: 8 to 16.
6. The method for preparing a water-in-oil rutin microemulsion as claimed in claim 2, wherein the temperature of heating and stirring in step 2 is 70-90 ℃.
7. The method for preparing a water-in-oil rutin microemulsion as claimed in claim 2, wherein the mass ratio of the phase A and the phase B in step 3 is 1: 0.01 to 0.1.
8. The method for preparing a water-in-oil rutin microemulsion as claimed in claim 2, wherein the conditions of the continuous shaking on the constant temperature oscillator in step 3 are as follows: the temperature is 20-30 ℃, and the time is 12-24 h.
CN202110869380.2A 2021-07-30 2021-07-30 Water-in-oil type rutin microemulsion and preparation method thereof Pending CN113546009A (en)

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CN104546712A (en) * 2014-12-26 2015-04-29 唯美度科技(北京)有限公司 Licoflavone alcohol-in-oil preparation and preparation method thereof
CN104606372A (en) * 2014-12-30 2015-05-13 唯美度科技(北京)有限公司 Tea polyphenol polyol-in-oil preparation and preparation method thereof
CN105979924A (en) * 2013-11-26 2016-09-28 科莱恩国际有限公司 Polyol-in-oil-emulsions for dermal delivery
CN108814995A (en) * 2018-06-28 2018-11-16 东南大学 A kind of non-aqueous multiple self-emulsifying systems of rutin and its preparation method and application

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KR20080022739A (en) * 2006-09-07 2008-03-12 주식회사 바이오랜드 A self-emulsifying carrier and the preparation method thereof
CN105979924A (en) * 2013-11-26 2016-09-28 科莱恩国际有限公司 Polyol-in-oil-emulsions for dermal delivery
CN104546712A (en) * 2014-12-26 2015-04-29 唯美度科技(北京)有限公司 Licoflavone alcohol-in-oil preparation and preparation method thereof
CN104606372A (en) * 2014-12-30 2015-05-13 唯美度科技(北京)有限公司 Tea polyphenol polyol-in-oil preparation and preparation method thereof
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Application publication date: 20211026