CN112972332B - Rose whitening essence and preparation method thereof - Google Patents

Rose whitening essence and preparation method thereof Download PDF

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Publication number
CN112972332B
CN112972332B CN202110233793.1A CN202110233793A CN112972332B CN 112972332 B CN112972332 B CN 112972332B CN 202110233793 A CN202110233793 A CN 202110233793A CN 112972332 B CN112972332 B CN 112972332B
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rose
mixing
extract
whitening
steps
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CN112972332A (en
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李培丰
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Aihua Aimei Beijing Biotechnology Co ltd
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爱花爱美(北京)生物科技有限公司
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    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL, OR TOILET PURPOSES
    • A61K8/00Cosmetics or similar toilet preparations
    • A61K8/18Cosmetics or similar toilet preparations characterised by the composition
    • A61K8/96Cosmetics or similar toilet preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution
    • A61K8/97Cosmetics or similar toilet 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]
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL, OR TOILET PURPOSES
    • A61K8/00Cosmetics or similar toilet preparations
    • A61K8/18Cosmetics or similar toilet preparations characterised by the composition
    • A61K8/30Cosmetics or similar toilet preparations characterised by the composition containing organic compounds
    • A61K8/31Hydrocarbons
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL, OR TOILET PURPOSES
    • A61K8/00Cosmetics or similar toilet preparations
    • A61K8/18Cosmetics or similar toilet preparations characterised by the composition
    • A61K8/30Cosmetics or similar toilet preparations characterised by the composition containing organic compounds
    • A61K8/33Cosmetics or similar toilet preparations characterised by the composition containing organic compounds containing oxygen
    • A61K8/36Carboxylic acids; Salts or anhydrides thereof
    • A61K8/361Carboxylic acids having more than seven carbon atoms in an unbroken chain; Salts or anhydrides thereof
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL, OR TOILET PURPOSES
    • A61K8/00Cosmetics or similar toilet preparations
    • A61K8/18Cosmetics or similar toilet preparations characterised by the composition
    • A61K8/30Cosmetics or similar toilet preparations characterised by the composition containing organic compounds
    • A61K8/60Sugars; Derivatives thereof
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL, OR TOILET PURPOSES
    • A61K8/00Cosmetics or similar toilet preparations
    • A61K8/18Cosmetics or similar toilet preparations characterised by the composition
    • A61K8/72Cosmetics or similar toilet preparations characterised by the composition containing organic macromolecular compounds
    • A61K8/84Cosmetics or similar toilet preparations characterised by the composition containing organic macromolecular compounds obtained by reactions otherwise than those involving only carbon-carbon unsaturated bonds
    • A61K8/89Polysiloxanes
    • A61K8/891Polysiloxanes saturated, e.g. dimethicone, phenyl trimethicone, C24-C28 methicone or stearyl dimethicone
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL, OR TOILET PURPOSES
    • A61K8/00Cosmetics or similar toilet preparations
    • A61K8/18Cosmetics or similar toilet 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 TOILET PURPOSES
    • A61K8/00Cosmetics or similar toilet preparations
    • A61K8/18Cosmetics or similar toilet preparations characterised by the composition
    • A61K8/96Cosmetics or similar toilet preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution
    • A61K8/97Cosmetics or similar toilet 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]
    • A61K8/9794Liliopsida [monocotyledons]
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61QSPECIFIC USE OF COSMETICS OR SIMILAR TOILET PREPARATIONS
    • A61Q19/00Preparations for care of the skin
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61QSPECIFIC USE OF COSMETICS OR SIMILAR TOILET PREPARATIONS
    • A61Q19/00Preparations for care of the skin
    • A61Q19/02Preparations for care of the skin for chemically bleaching or whitening the skin
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61QSPECIFIC USE OF COSMETICS OR SIMILAR TOILET PREPARATIONS
    • A61Q19/00Preparations for care of the skin
    • A61Q19/08Anti-ageing preparations
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL, OR TOILET PURPOSES
    • A61K2800/00Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
    • A61K2800/40Chemical, physico-chemical or functional or structural properties of particular ingredients
    • A61K2800/59Mixtures
    • A61K2800/592Mixtures of compounds complementing their respective functions
    • A61K2800/5922At least two compounds being classified in the same subclass of A61K8/18
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL, OR TOILET PURPOSES
    • A61K2800/00Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
    • A61K2800/74Biological properties of particular ingredients
    • A61K2800/78Enzyme modulators, e.g. Enzyme agonists
    • A61K2800/782Enzyme inhibitors; Enzyme antagonists
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL, OR TOILET 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
    • A61K2800/805Corresponding aspects not provided for by any of codes A61K2800/81 - A61K2800/95
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL, OR TOILET 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

Abstract

The invention discloses rose whitening essence and a preparation method thereof, wherein deionized water, a cosolvent, a whitening agent, a softening agent, an emulsifier, a pH regulator and a preservative are mixed and homogenized to obtain mixed liquid; and mixing the mixed solution and a thickening agent and homogenizing to obtain the rose whitening essence. The rose whitening essence obtained by the specific method can effectively remove free radicals, improve the immunity of skin, reduce inflammation and sensitivity, reduce the content of red pigment, ensure that the whole appearance of the skin is transparent, bright, white and shiny, promote the metabolism of the generated melanin, has stronger inhibition effect on tyrosinase, simultaneously acts at the source end and the route end of the melanin, further reduces the content of the melanin in the skin, and further improves the whiteness and the brightness of the skin.

Description

Rose whitening essence and preparation method thereof
Technical Field
The invention relates to the technical field of whitening essence, in particular to rose whitening essence and a preparation method thereof.
Background
Roses (Rose rugosa Thumb.) are perennial evergreen or deciduous shrubs of the genus rosa of the family rosaceae and are widely grown worldwide. The roses have the functions of eating and health care, and are officially approved by the state as new resource food in 2010. Modern medicine shows that roses contain more than 300 chemical components, and the roses contain flavonoid compounds which have antioxidant activity and can reduce and eliminate free radicals. The plant flavonoid compound not only can eliminate free radicals in human bodies, but also can inhibit the generation of free radicals, has the effects of preventing aging, cardiovascular diseases, cancers and the like, is an effective antioxidant, and is widely applied to the industries of foods, medical health products, cosmetics and the like. Text of materia medica (text of materia medica) Zhongdao: "Rose flower, clear but not turbid, and not fierce, liver softening and stomach awaking, qi-flowing and blood circulation promoting, and dredging and suffocating without the disadvantage of pungent, warm and hard dryness, among the qi-pushing-off and medicine-dividing, it is most quick and most tame, fragrant, so there is no way to match. The rose contains more than 300 chemical components, such as aromatic alcohol, aldehyde, fatty acid, phenol and oil and fat containing essence, and the rose product is usually eaten to soften liver and wake stomach, relax qi and activate blood, maintain beauty and keep young and refresh people. The flowers and roots of the rose can be used as medicine, has the functions of regulating qi, promoting blood circulation, astringing and the like, and is mainly used for treating irregular menstruation, traumatic injury, liver qi and stomach pain, breast swelling and pain and other symptoms. The rose pulp can be made into jam, has special flavor, contains abundant vitamin C and vitamin P, and can be used for preventing acute and chronic infectious diseases, coronary heart disease, liver disease, carcinogen generation and metastasis, etc. The rose essential oil (called rose dew) extracted from rose petal by distillation method can also improve skin texture, and promote blood circulation and metabolism. The current utilization of roses has the problems of low acquisition rate, insufficient activity maintenance of effective components and the like during filter pressing.
Disclosure of Invention
Aiming at the defects in the prior art, the invention provides rose whitening essence and a preparation method thereof.
In order to solve the technical problems, the invention adopts the technical scheme that:
a rose whitening essence comprises deionized water, cosolvent, thickener, whitening agent, emollient, emulsifier, pH regulator, and antiseptic.
The preparation method of the cosolvent comprises the following steps: and mixing absolute ethyl alcohol, glycerol, propylene carbonate and 1, 3-butanediol, and homogenizing to obtain the cosolvent.
Preferably, the preparation method of the cosolvent comprises the following steps: mixing absolute ethyl alcohol, glycerol, propylene carbonate and 1, 3-butanediol according to the mass ratio of (26.3-28.9): (10.5-14.6): (6.3-8.2): 4.9-6.2) at 18-22 ℃, and carrying out homogenization treatment at the rotating speed of 14000-charge 16000rpm for 1.5-3min to obtain the cosolvent.
Most preferably, the preparation method of the cosolvent comprises the following steps: mixing absolute ethyl alcohol, glycerol, propylene carbonate and 1, 3-butanediol according to the mass ratio of 27.2:13.1:7.6:5.8 at 20 ℃, and carrying out homogenization treatment at the rotating speed of 15000rpm for 2min to obtain the cosolvent.
The preparation method of the thickening agent comprises the following steps: mixing trehalose, betaine, linoleic acid and absolute ethyl alcohol, and stirring to obtain the thickening agent.
Preferably, the preparation method of the thickening agent comprises the following steps: mixing trehalose, betaine, linoleic acid and absolute ethyl alcohol according to the mass ratio of (10.3-13.1): (4.6-6.1): (3.1-4.2): 17.9-19.5) at 18-22 ℃, and stirring at the rotation speed of 1000-.
Most preferably, the thickener is prepared by the following method: mixing trehalose, betaine, linoleic acid and absolute ethyl alcohol according to the mass ratio of 11.7:5.3:3.8:18.1 at 20 ℃, and stirring at the rotating speed of 1200rpm for 15min to obtain the thickening agent.
The preparation method of the whitening agent comprises the following steps: mixing the rose extract, the iris tonkinensis root extract, the sage herb extract, the Sudan cola seed extract and 1, 3-butanediol, and homogenizing to obtain the whitening agent.
Preferably, the preparation method of the whitening agent comprises the following steps: mixing the rose extract, the iris tonkinensis root extract, the salvia miltiorrhiza bunge extract, the sudan cola seed extract and the 1, 3-butanediol according to the mass ratio of (65.6-70.2): (15.7-17.1): (13.9-16.3): (5.2-8.3): 198.1-219.3 at 18-22 ℃, and homogenizing at the rotation speed of 14000 and 16000rpm for 1.5-3min to obtain the whitening agent.
Most preferably, the preparation method of the whitening agent comprises the following steps: mixing the rose extract, the iris tonkinensis root extract, the sage extract, the Sudan cola nut extract and the 1, 3-butanediol according to the mass ratio of 67.3:16.3:15.7:7.1:201.2 at 20 ℃, and homogenizing at the rotating speed of 15000rpm for 2min to obtain the whitening agent.
The preparation method of the softening agent comprises the following steps: mixing and homogenizing cyclohexasiloxane, polydimethylsiloxane, squalane and 1, 3-butanediol to obtain the softening agent.
Preferably, the preparation method of the softening agent comprises the following steps: mixing the cyclohexasiloxane, the polydimethylsiloxane, the squalane and the 1, 3-butanediol according to the mass ratio of (16.8-22.9) to (11.9-17.6) to (8.7-12.2) to (59.2-75.3) at 18-22 ℃, and homogenizing at the rotating speed of 14000-.
Most preferably, the preparation method of the emollient comprises the following steps: mixing the cyclohexasiloxane, the polydimethylsiloxane, the squalane and the 1, 3-butanediol according to the mass ratio of 19.1:13.5:9.8:68.6 at 20 ℃, and homogenizing at the rotating speed of 15000rpm for 2min to obtain the softening agent.
The preparation method of the emulsifier comprises the following steps: mixing isocetyl polyether-10, PPG-6-decyltetradecyl polyether-20 and anhydrous ethanol, and homogenizing to obtain the emulsifier.
Preferably, the preparation method of the emulsifier comprises the following steps: isocetyl polyether-10, PPG-6-decyltetradecyl polyether-20 and absolute ethyl alcohol are mixed according to the mass ratio of (11.9-19.7) to (2.3-7.1) to (41.2-53.7) at the temperature of 18-22 ℃ and are homogenized at the rotating speed of 14000-.
Most preferably, the preparation method of the emulsifier comprises the following steps: isocetyl polyether-10, PPG-6-decyltetradecyl polyether-20 and absolute ethyl alcohol were mixed at a mass ratio of 13.8:4.7:43.2 at 20 ℃ and homogenized at 15000rpm for 2min to obtain the emulsifier.
The preparation method of the pH regulator comprises the following steps: and mixing and stirring dipotassium phosphate, sodium bicarbonate, potassium hydroxide and deionized water to obtain the pH regulator.
Preferably, the preparation method of the pH regulator comprises the following steps: at the temperature of 18-22 ℃, mixing dipotassium hydrogen phosphate, sodium bicarbonate, potassium hydroxide and deionized water according to the mass ratio of (7.8-12.6): (3.1-5.2): (1.8-4.5): 28.8-40.3, and stirring at the rotating speed of 1000-.
Most preferably, the preparation method of the pH regulator comprises the following steps: and mixing dipotassium phosphate, sodium bicarbonate, potassium hydroxide and deionized water according to the mass ratio of 9.1:3.3:2.7:31.9 at 20 ℃, and stirring at the rotating speed of 1200rpm for 10min to obtain the pH regulator.
The preparation method of the preservative comprises the following steps: and mixing potassium sorbate, sodium metabisulfite and deionized water, and stirring to obtain the preservative.
Preferably, the preparation method of the preservative comprises the following steps: mixing potassium sorbate, sodium pyrosulfite and deionized water according to the mass ratio of (1.6-4.6) to (0.1-1.7) to (8.2-20.3), and stirring at the rotation speed of 1000-1500rpm for 6-9min to obtain the preservative.
Most preferably, the preparation method of the preservative comprises the following steps: mixing potassium sorbate, sodium metabisulfite and deionized water according to the mass ratio of 1.7:1.2:10.3, and stirring at the rotating speed of 1200rpm for 8min to obtain the preservative.
The preparation method of the rose extract comprises the following steps:
firstly, rose petals, an ethanol water solution and a penetration enhancer are mixed and stirred, and meanwhile, ultrasonic treatment is carried out to obtain rose soaking matter; the penetration enhancer is one or a mixture of two of litsea cubeba oil and lemongrass oil;
filtering the rose soaked substance obtained in the step I to obtain filtrate, centrifuging the filtrate, and collecting supernatant;
thirdly, concentrating the supernatant obtained in the second step to obtain a concentrated solution;
fourthly, mixing and stirring the concentrated solution obtained in the third step with absolute ethyl alcohol, and simultaneously carrying out ultrasonic treatment to obtain a concentrated solution-absolute ethyl alcohol mixture;
regulating the pH of the concentrated solution-absolute ethyl alcohol mixture obtained in the step (iv) by using malic acid, standing, then performing centrifugal treatment, taking the precipitate, and drying the precipitate to obtain a rose crude extract;
sixthly, soaking FL-2 type macroporous adsorption resin in an ethanol water solution, then washing the resin with the ethanol water solution until no white turbidity exists after the ethanol eluent is mixed with water, and then filling the washed resin into a column;
seventhly, mixing the rose crude extract obtained in the fifth step with an ethanol water solution and stirring to obtain a rose crude extract-ethanol water solution;
eighthly, loading the rose crude extract-ethanol water solution obtained in the step seven; then, washing with distilled water and ethanol water solution successively to remove impurities; collecting high-purity eluent;
ninthly, freeze-drying the high-purity eluent obtained in the step (viii) until powdery solid is obtained, namely the rose extract.
Preferably, the preparation method of the rose extract comprises the following steps:
firstly, rose petals, 72-76 wt.% ethanol aqueous solution and a penetration enhancer are mixed according to the mass ratio of (4-6) to (0.8-1.3) at 22-26 ℃, and are stirred for 18-22h at the rotating speed of 360rpm, and ultrasonic treatment with the power of 380-450w and the frequency of 36-45kHz is simultaneously used to obtain rose soaking substances; the penetration enhancer is a mixture of litsea cubeba oil and lemongrass oil according to the mass ratio of (1-4) to (1-4);
secondly, carrying out filter pressing on the rose soaked substance obtained in the step I for 40-60min by adopting the pressure of 0.9-1.2MPa to obtain a filtrate, centrifuging the filtrate for 18-26min at the rotating speed of 4800-5500rpm, and collecting the supernatant;
③ concentrating the supernatant obtained in the step (II) to 48-53 percent of the volume of the original supernatant under the conditions of (-55) - (-48) DEG C and 8-11kPa to obtain concentrated solution;
fourthly, mixing the concentrated solution obtained in the third step with absolute ethyl alcohol at the temperature of 22-26 ℃, stirring for 30-50min at the rotating speed of 360rpm, and simultaneously performing ultrasonic treatment with the power of 380 plus 450w and the frequency of 36-45kHz to obtain a concentrated solution-absolute ethyl alcohol mixture; the concentration of absolute ethanol in the concentrate-absolute ethanol mixture is 78-81 wt.%;
fifthly, regulating the pH value of the concentrated solution-absolute ethyl alcohol mixture obtained in the step (d) to 2.8-3.2 by using malic acid at the temperature of 22-26 ℃, standing for 28-34h at the temperature of 2-5 ℃, centrifuging for 20-27min at the temperature of 2-5 ℃ at the rotating speed of 4800 + 5500rpm, taking the precipitate, and drying the precipitate at the temperature of 5-7 ℃ to obtain a rose crude extract;
sixthly, soaking FL-2 type macroporous adsorption resin for 13-18h at 22-26 ℃ by using an ethanol aqueous solution with the concentration of 12-18 wt.%, then washing the resin by using the ethanol aqueous solution with the concentration of 12-18 wt.% until the ethanol eluent is mixed with water without white turbidity, and then packing the washed resin into a column according to the ratio of the diameter of the resin to the height of the column of 1 (8-10);
seventhly, mixing the rose crude extract obtained in the step (V) with an ethanol water solution with the concentration of 78-82 wt.% according to the mass ratio of (0.8-1.3) to (900-;
eighthly, loading the rose crude extract-ethanol aqueous solution obtained in the step (c) at 22-26 ℃, wherein the loading amount is 12-16% of the weight of the resin, the loading flow rate is (0.8-0.95) mL/min, and the standing time is 22-28 min; then, respectively washing with distilled water and 72-76 wt.% ethanol water solution to remove impurities; the mass ratio of the distilled water to the resin is (4-6) to (0.8-1.3); the mass ratio of the 72-76 wt.% ethanol aqueous solution to the resin is (4-6): 0.8-1.2); the washing flow rate is (28-32) mL/min, the elution flow rate is (36-40) mL/min, and high-purity eluent is collected;
ninthly, freeze-drying the high-purity eluent obtained in the step (b) at the temperature of between (-52) and (-48) DEG C under the air pressure of between 9 and 11kPa until powdery solid is obtained, namely the rose extract.
Most preferably, the preparation method of the rose extract comprises the following steps:
firstly, rose petals, 75 wt.% ethanol water solution and a penetration enhancer are mixed according to the mass ratio of 5:5:1 at 25 ℃, stirred for 20 hours at the rotating speed of 300rpm, and simultaneously treated by ultrasonic waves with the power of 400w and the frequency of 42kHz to obtain rose soaking substances; the penetration enhancer is a mixture of litsea cubeba oil and lemongrass oil according to the mass ratio of 1: 1;
secondly, carrying out pressure filtration on the rose soaked substance obtained in the first step for 45min by adopting the pressure of 1MPa to obtain a filtrate, centrifuging the filtrate for 25min at the rotating speed of 5000rpm, and collecting a supernatant;
thirdly, concentrating the supernatant obtained in the second step to 50 percent of the volume of the original supernatant under the conditions of-50 ℃ and 10kPa to obtain concentrated solution;
fourthly, mixing the concentrated solution obtained in the third step with absolute ethyl alcohol at 25 ℃, stirring for 40min at the rotating speed of 300rpm, and simultaneously treating with ultrasonic waves with the power of 400w and the frequency of 42kHz to obtain a concentrated solution-absolute ethyl alcohol mixture; the concentration of absolute ethanol in the concentrate-absolute ethanol mixture was 80 wt.%;
fifthly, regulating the pH value of the concentrated solution-absolute ethyl alcohol mixture obtained in the step (iv) to 3 by using malic acid at 25 ℃, standing for 30 hours at 3 ℃, then centrifuging for 25 minutes at 3 ℃ at 5000rpm, taking the precipitate, and drying the precipitate at 65 ℃ to obtain a rose crude extract;
soaking FL-2 macroporous adsorbent resin in 15 wt.% ethanol water solution at 25 deg.C for 15h, washing the resin with 15 wt.% ethanol water solution until the ethanol eluate is mixed with water and there is no white turbidity, and packing the washed resin into column according to the ratio of resin diameter to column height of 1: 9;
seventhly, mixing the rose crude extract obtained in the fifth step with 80 wt.% aqueous solution of ethanol according to the mass ratio of 1:1000, and stirring at the rotating speed of 300rpm for 20min to obtain the rose crude extract-aqueous solution of ethanol;
eighthly, loading the rose crude extract-ethanol aqueous solution obtained in the step (seventhly) at 25 ℃, wherein the loading amount is 15 percent of the weight of the resin, the loading flow rate is 0.85mL/min, and the standing time is 25 min; then, washing with distilled water and 75 wt.% ethanol water solution to remove impurities; the mass ratio of the distilled water to the resin is 5: 1; the mass ratio of the ethanol aqueous solution with the concentration of 75 wt.% to the resin is 5: 1; the washing flow rate is 30mL/min, the elution flow rate is 38mL/min, and high-purity eluent is collected;
ninthly, freeze-drying the high-purity eluent obtained in the step (b) at the temperature of 50 ℃ below zero and under the air pressure of 10kPa until powder solid is obtained, namely the rose extract.
The preparation method of the rose whitening essence comprises the following steps: mixing and homogenizing the deionized water, the cosolvent, the whitening agent, the softening agent, the emulsifier, the pH regulator and the preservative to obtain a mixed solution; and mixing the mixed solution and the thickening agent and homogenizing to obtain the rose whitening essence.
Preferably, the preparation method of the rose whitening essence comprises the following steps: mixing the deionized water, the cosolvent, the whitening agent, the emollient, the emulsifier, the pH regulator and the preservative, and homogenizing at the rotating speed of 14000-; the concentrations of the cosolvent, the whitening agent, the emollient, the emulsifier, the pH regulator and the preservative are (31.8-34.5) wt.%, from (10.5-12.7) wt.%, from (1.5-2.1) wt.%, from (0.9-1.6) wt.%, from (0.5-0.8) wt.% and from (0.4-0.6) wt.%, and the balance is deionized water; mixing the mixed solution and the thickening agent according to the mass ratio of (96.6-97.0) to (3.0-3.4), and homogenizing at the rotating speed of 14000-16000rpm at 18-22 ℃ for 2-4min to obtain the rose whitening essence.
Most preferably, the preparation method of the rose whitening essence comprises the following steps: mixing the deionized water, the cosolvent, the whitening agent, the softening agent, the emulsifier, the pH regulator and the preservative, and homogenizing at the rotating speed of 15000rpm at 20 ℃ for 3min to obtain a mixed solution; the concentrations of the cosolvent, the whitening agent, the emollient, the emulsifier, the pH regulator and the preservative are 33.2 wt.%, 11.3 wt.%, 1.7 wt.%, 1.2 wt.%, 0.7 wt.% and 0.5 wt.%, respectively, and the balance is deionized water; and mixing the mixed solution and the thickening agent according to a mass ratio of 96.8:3.2, and homogenizing at the rotating speed of 15000rpm at 20 ℃ for 3min to obtain the rose whitening essence.
The rose extract contains a large amount of rose total flavonoids which are active ingredients with various beautifying effects of removing free radicals, resisting inflammation, resisting oxidation, removing yellow, brightening, resisting wrinkles, fading spots and the like, can improve the skin state after long-term use, and presents tender, white and bright water. The litsea cubeba oil and the lemongrass oil are rich in solvents with active chemical properties, such as alpha-lupinene, alpha-pinene and the like, can effectively promote the rose total flavonoids to seep out of cells of the rose, and improve the collection rate of the filtrate obtained by medium-pressure filtration of the rose soak solution; when the rose extract and the rose flavone are compounded for use, the rose total flavone can be promoted to exude, and simultaneously, the antioxidant protection effect is achieved, and the rose extract with higher rose total flavone content and stronger active ingredient activity can be obtained. The active ingredients of the vetiver iris root extract, the salvia miltiorrhiza bunge extract, the sudan cola seed extract, squalane, trehalose, linoleic acid, polydimethylsiloxane and the like can improve the immunity of the skin and reduce the occurrence of inflammation and sensitivity phenomena, thereby reducing the content of red pigment and leading the whole appearance of the skin to be transparent, bright, white and shiny. The active antioxidant components such as total flavonoids in the rose extract prepared by the specific method can effectively remove free radicals, promote the metabolism of generated melanin, have strong inhibition effect on tyrosinase, simultaneously take effect at the two ends of the source and the route of the melanin, further reduce the content of the melanin in the skin and further improve the whiteness and the brightness of the skin.
The invention has the beneficial effects that: the rose whitening essence obtained by the specific method of the invention effectively removes free radicals, improves the skin immunity, reduces inflammation and sensitivity, reduces the content of red pigment, enables the whole skin to be transparent and bright, white and shiny, promotes the metabolism of the generated melanin, has stronger inhibition effect on tyrosinase, simultaneously takes effect at the source and the route of the melanin, further reduces the content of the melanin in the skin, and further improves the whiteness and the brightness of the skin.
Detailed Description
The above summary of the present invention is described in further detail below with reference to specific embodiments, but it should not be understood that the scope of the above subject matter of the present invention is limited to the following examples.
Introduction of some raw materials in this application:
absolute ethanol, CAS: 64-17-5, available from Nanjing chemical reagents, Inc., under the trade designation: c0692035010, specification: EP, molecular weight: 46.07. the function is as follows: a solvent. The content of the rose whitening essence is more than 14.61 wt.%.
Glycerol, CAS: 56-81-5, available from Nanjing Chemicals GmbH, under trade designation: c0690510224, specification: AR, molecular weight: 92.09. the function is as follows: solvent and humectant. The rose whitening essence comprises 5.996-9.378 wt.%.
Propylene carbonate, CAS: 51260-39-0, available from sahn chemical technology (shanghai) ltd, under trade designation: a020006-100g, purity: 99.0%, molecular weight: 102.09. the function is as follows: solvent, viscosity control agent. The rose whitening essence comprises 3.456-5.499 wt.%.
1, 3-butanediol, CAS: 107-88-0, available from western chemistry technologies (Shandong) Ltd, under trade designation: b15109-500g, Specification: 99.0%, molecular weight: 90.12. the function is as follows: solvent and humectant, increase smoothness of product, and inhibit bacteria. The content of the rose whitening essence is more than 2.659 wt.%.
Trehalose, CAS: 99-20-7, available from western chemistry technologies (Shandong) Ltd, under trade designation: a14775-500g, specification: 99.0%, molecular weight: 342.30. the function is as follows: thickening agent, humectant and stabilizer. The rose whitening essence comprises 0.7705-1.1509 wt.%.
Betaine, CAS: 107-43-7, available from western chemical technology, Shandong, Inc., under the trade designation: b11244-500g, specification: 99.0%, molecular weight: 117.15. the function is as follows: thickening agent and humectant. The content of the rose whitening essence is 0.3333-0.5545 wt.%.
Linoleic acid, CAS: 60-33-3, available from western chemistry technologies (Shandong) Ltd, under trade designation: a16095-500ml, specification: 95.0%, molecular weight: 280.46. the function is as follows: thickening agent, humectant, repairing skin injury, and keeping skin elasticity. The rose whitening essence comprises 0.2225-0.3859 wt.%.
Vetiver iris root extract, CAS: 90045-89-9, purchased from Gansu Probiotics Biotech limited, purity: 98.0%, extract source: rhizoma Iridis Tectori (IRIS FLORENTINA). The function is as follows: enhancing metabolism of skin cells, resisting aging, relieving inflammation, and whitening skin. The rose whitening essence comprises 0.4829-0.7024 wt.%.
Sage extract, CAS: 8022-56-8, available from welength technologies ltd, purity: 98.0%, extract source: salvia OFFICINALIS (Salvia OFFICINALIS). The function is as follows: tranquilizing, relieving, antiinflammatory, reducing oil secretion, and tightening skin. The rose whitening essence comprises 0.4288-0.6673 wt.%.
Sudan cola seed extract, CAS: 89997-82-0, available from Ningxia vanilla Biotechnology Ltd, purity: 98.0%, extract source: sudan COLA nut (COLA ACUMINATA). The function is as follows: improving skin cell activity, whitening skin, and inhibiting bacteria. The rose whitening essence comprises 0.1608-0.3390 wt.%.
Cyclohexasiloxane, CAS: 540-97-6, available from carbofuran technologies ltd, under the trade designation: 9687.12-10MG, purity: 97.0%, molecular weight: 445. the function is as follows: smoothing agent, improving product ductility, improving skin feeling, and moistening agent. The rose whitening essence comprises 0.2005-0.4542 wt.%.
Polydimethylsiloxane, CAS: 9006-65-9, available from western chemical technology, Shandong, Inc., under the trade designation: a15581-100g, specification: and AR. The function is as follows: promoting penetration and improving skin softness. The rose whitening essence comprises 0.1420-0.3505 wt.%.
Squalane, CAS: 111-01-3, available from west asia chemical technology (shandong) ltd, under the trade designation: b14680-500ml, specification: 98.0%, molecular weight: 422.81. the function is as follows: the lubricant can improve skin softness and promote penetration. The content of the rose whitening essence is 0.1013-0.2483 wt.%.
Isocetylpolyether-10, CAS: 69364-63-2, available from Nantong Chen Runji chemical Co., Ltd, purity: 98.0 percent. The function is as follows: an emulsifier. The rose whitening essence comprises 0.1423-0.4838 wt.%.
PPG-6-decyltetradecanol polyether-20, CAS: 72484-69-6, available from Nantong Chen Runji chemical Co., Ltd, purity: 98.0 percent. The function is as follows: an emulsifier. The content of the rose whitening essence is 0.0264-0.1516 wt.%.
Dipotassium phosphate, CAS: 7758-11-4, available from chemical technology, west asia (Shandong) Ltd, under trade designation: b62544-500g, Specification: GR, molecular weight: 174.18. the function is as follows: a buffering agent. The content of the rose whitening essence is 0.0652-0.2112 wt.%.
Sodium bicarbonate, CAS: 144-55-8, available from western chemistry technologies (Shandong) Ltd, under trade designation: c10227-500g, Specification: AR, molecular weight: 84.01. the function is as follows: a buffering agent. The content of the rose whitening essence is 0.0398-0.0926 wt.%.
Potassium hydroxide, CAS: 1310-58-3, available from west asia chemical technology (shandong) ltd, under the trade designation: b10105-500g, specification: 95.0%, molecular weight: 56.11. the function is as follows: a buffering agent. The content of the rose whitening essence is 0.0145-0.0790 wt.%.
Potassium sorbate, CAS: 24634-61-5, available from western chemical technology, Shandong, Inc., under trade designation: a12216-500g, Specification: AR, molecular weight: 150.21. the function is as follows: and (4) a preservative. The content of the rose whitening essence is 0.0262-0.2075 wt.%.
Sodium metabisulfite, CAS: 7681-57-4 available from west asia chemical technology (Shandong) Ltd, under trade designation: b12071-500g, specification: AR, molecular weight: 190.11. the function is as follows: preservative and grease-resistant oxidant. The content of the rose whitening essence is 0.0023-0.0860 wt.%.
Rose, variety: damascus rose purchased from Kunsheng flower nursery stock Limited, Qingzhou city.
Litsea cubeba oil, CAS: 68855-99-2, available from Shanghai-derived leaf Biotech, Inc., under trade designation: s25515-500 ml. The function is as follows: and (5) promoting infiltration.
Lemon grass oil, CAS: 8007-02-1, available from Hubei Nonakojic technologies, purity: 98.0 percent. The function is as follows: and (5) promoting infiltration.
Malic acid, CAS: 97-67-6, available from western chemistry technologies (Shandong) Ltd, under trade designation: a11100-500g, purity: 99.0%, molecular weight: 134.09. the function is as follows: the pH is adjusted during the preparation of the rose extract.
FL-2 type macroporous adsorption resin, available from Tianjin Kaishi resin science and technology Limited. The function is as follows: adsorbing, washing and removing impurities.
The content of the rose extract prepared by the specific method in the rose whitening essence is 2.037-2.853 wt.%.
Example 1
A rose whitening essence comprises deionized water, cosolvent, thickener, whitening agent, emollient, emulsifier, pH regulator, and antiseptic.
The preparation method of the cosolvent comprises the following steps: mixing absolute ethyl alcohol, glycerol, propylene carbonate and 1, 3-butanediol according to the mass ratio of 27.2:13.1:7.6:5.8 at 20 ℃, and carrying out homogenization treatment at the rotating speed of 15000rpm for 2min to obtain the cosolvent.
The preparation method of the thickening agent comprises the following steps: mixing trehalose, betaine, linoleic acid and absolute ethyl alcohol according to the mass ratio of 11.7:5.3:3.8:18.1 at 20 ℃, and stirring at the rotating speed of 1200rpm for 15min to obtain the thickening agent.
The preparation method of the whitening agent comprises the following steps: mixing the rose extract, the iris tonkinensis root extract, the sage extract, the Sudan cola nut extract and the 1, 3-butanediol according to the mass ratio of 67.3:16.3:15.7:7.1:201.2 at 20 ℃, and homogenizing at the rotating speed of 15000rpm for 2min to obtain the whitening agent.
The preparation method of the softening agent comprises the following steps: mixing the cyclohexasiloxane, the polydimethylsiloxane, the squalane and the 1, 3-butanediol according to the mass ratio of 19.1:13.5:9.8:68.6 at 20 ℃, and homogenizing at the rotating speed of 15000rpm for 2min to obtain the softening agent.
The preparation method of the emulsifier comprises the following steps: isocetyl polyether-10, PPG-6-decyltetradecyl polyether-20 and absolute ethyl alcohol were mixed at a mass ratio of 13.8:4.7:43.2 at 20 ℃ and homogenized at 15000rpm for 2min to obtain the emulsifier.
The preparation method of the pH regulator comprises the following steps: and mixing dipotassium phosphate, sodium bicarbonate, potassium hydroxide and deionized water according to the mass ratio of 9.1:3.3:2.7:31.9 at 20 ℃, and stirring at the rotating speed of 1200rpm for 10min to obtain the pH regulator.
The preparation method of the preservative comprises the following steps: mixing potassium sorbate, sodium metabisulfite and deionized water according to the mass ratio of 1.7:1.2:10.3, and stirring at the rotating speed of 1200rpm for 8min to obtain the preservative.
The preparation method of the rose extract comprises the following steps:
firstly, rose petals, 75 wt.% ethanol water solution and a penetration enhancer are mixed according to the mass ratio of 5:5:1 at 25 ℃, stirred for 20 hours at the rotating speed of 300rpm, and simultaneously treated by ultrasonic waves with the power of 400w and the frequency of 42kHz to obtain rose soaking substances; the penetration enhancer is a mixture of litsea cubeba oil and lemongrass oil according to the mass ratio of 1: 1;
secondly, carrying out pressure filtration on the rose soaked substance obtained in the first step for 45min by adopting the pressure of 1MPa to obtain a filtrate, centrifuging the filtrate for 25min at the rotating speed of 5000rpm, and collecting a supernatant;
thirdly, concentrating the supernatant obtained in the second step to 50 percent of the volume of the original supernatant under the conditions of-50 ℃ and 10kPa to obtain concentrated solution;
fourthly, mixing the concentrated solution obtained in the third step with absolute ethyl alcohol at 25 ℃, stirring for 40min at the rotating speed of 300rpm, and simultaneously treating with ultrasonic waves with the power of 400w and the frequency of 42kHz to obtain a concentrated solution-absolute ethyl alcohol mixture; the concentration of absolute ethanol in the concentrate-absolute ethanol mixture was 80 wt.%;
fifthly, regulating the pH value of the concentrated solution-absolute ethyl alcohol mixture obtained in the step (iv) to 3 by using malic acid at 25 ℃, standing for 30 hours at 3 ℃, then centrifuging for 25 minutes at 3 ℃ at 5000rpm, taking the precipitate, and drying the precipitate at 65 ℃ to obtain a rose crude extract;
soaking FL-2 macroporous adsorbent resin in 15 wt.% ethanol water solution at 25 deg.C for 15h, washing the resin with 15 wt.% ethanol water solution until the ethanol eluate is mixed with water and there is no white turbidity, and packing the washed resin into column according to the ratio of resin diameter to column height of 1: 9;
seventhly, mixing the rose crude extract obtained in the fifth step with 80 wt.% aqueous solution of ethanol according to the mass ratio of 1:1000, and stirring at the rotating speed of 300rpm for 20min to obtain the rose crude extract-aqueous solution of ethanol;
eighthly, loading the rose crude extract-ethanol aqueous solution obtained in the step (seventhly) at 25 ℃, wherein the loading amount is 15 percent of the weight of the resin, the loading flow rate is 0.85mL/min, and the standing time is 25 min; then, washing with distilled water and 75 wt.% ethanol water solution to remove impurities; the mass ratio of the distilled water to the resin is 5: 1; the mass ratio of the ethanol aqueous solution with the concentration of 75 wt.% to the resin is 5: 1; the washing flow rate is 30mL/min, the elution flow rate is 38mL/min, and high-purity eluent is collected;
ninthly, freeze-drying the high-purity eluent obtained in the step (b) at the temperature of 50 ℃ below zero and under the air pressure of 10kPa until powder solid is obtained, namely the rose extract.
The preparation method of the rose whitening essence comprises the following steps: mixing the deionized water, the cosolvent, the whitening agent, the softening agent, the emulsifier, the pH regulator and the preservative, and homogenizing at the rotating speed of 15000rpm at 20 ℃ for 3min to obtain a mixed solution; the concentrations of the cosolvent, the whitening agent, the emollient, the emulsifier, the pH regulator and the preservative are 33.2 wt.%, 11.3 wt.%, 1.7 wt.%, 1.2 wt.%, 0.7 wt.% and 0.5 wt.%, respectively, and the balance is deionized water; and mixing the mixed solution and the thickening agent according to a mass ratio of 96.8:3.2, and homogenizing at the rotating speed of 15000rpm at 20 ℃ for 3min to obtain the rose whitening essence.
Example 2
A rose whitening essence comprises deionized water, cosolvent, thickener, whitening agent, emollient, emulsifier, pH regulator, and antiseptic.
The preparation method of the cosolvent comprises the following steps: mixing absolute ethyl alcohol, glycerol, propylene carbonate and 1, 3-butanediol according to the mass ratio of 27.2:13.1:7.6:5.8 at 20 ℃, and carrying out homogenization treatment at the rotating speed of 15000rpm for 2min to obtain the cosolvent.
The preparation method of the thickening agent comprises the following steps: mixing trehalose, betaine, linoleic acid and absolute ethyl alcohol according to the mass ratio of 11.7:5.3:3.8:18.1 at 20 ℃, and stirring at the rotating speed of 1200rpm for 15min to obtain the thickening agent.
The preparation method of the whitening agent comprises the following steps: mixing the rose extract, the iris tonkinensis root extract, the sage extract, the Sudan cola nut extract and the 1, 3-butanediol according to the mass ratio of 67.3:16.3:15.7:7.1:201.2 at 20 ℃, and homogenizing at the rotating speed of 15000rpm for 2min to obtain the whitening agent.
The preparation method of the softening agent comprises the following steps: mixing the cyclohexasiloxane, the polydimethylsiloxane, the squalane and the 1, 3-butanediol according to the mass ratio of 19.1:13.5:9.8:68.6 at 20 ℃, and homogenizing at the rotating speed of 15000rpm for 2min to obtain the softening agent.
The preparation method of the emulsifier comprises the following steps: isocetyl polyether-10, PPG-6-decyltetradecyl polyether-20 and absolute ethyl alcohol were mixed at a mass ratio of 13.8:4.7:43.2 at 20 ℃ and homogenized at 15000rpm for 2min to obtain the emulsifier.
The preparation method of the pH regulator comprises the following steps: and mixing dipotassium phosphate, sodium bicarbonate, potassium hydroxide and deionized water according to the mass ratio of 9.1:3.3:2.7:31.9 at 20 ℃, and stirring at the rotating speed of 1200rpm for 10min to obtain the pH regulator.
The preparation method of the preservative comprises the following steps: mixing potassium sorbate, sodium metabisulfite and deionized water according to the mass ratio of 1.7:1.2:10.3, and stirring at the rotating speed of 1200rpm for 8min to obtain the preservative.
The preparation method of the rose extract comprises the following steps:
firstly, rose petals, 75 wt.% ethanol water solution and a penetration enhancer are mixed according to the mass ratio of 5:5:1 at 25 ℃, stirred for 20 hours at the rotating speed of 300rpm, and simultaneously treated by ultrasonic waves with the power of 400w and the frequency of 42kHz to obtain rose soaking substances; the penetration enhancer is litsea cubeba oil;
secondly, carrying out pressure filtration on the rose soaked substance obtained in the first step for 45min by adopting the pressure of 1MPa to obtain a filtrate, centrifuging the filtrate for 25min at the rotating speed of 5000rpm, and collecting a supernatant;
thirdly, concentrating the supernatant obtained in the second step to 50 percent of the volume of the original supernatant under the conditions of-50 ℃ and 10kPa to obtain concentrated solution;
fourthly, mixing the concentrated solution obtained in the third step with absolute ethyl alcohol at 25 ℃, stirring for 40min at the rotating speed of 300rpm, and simultaneously treating with ultrasonic waves with the power of 400w and the frequency of 42kHz to obtain a concentrated solution-absolute ethyl alcohol mixture; the concentration of absolute ethanol in the concentrate-absolute ethanol mixture was 80 wt.%;
fifthly, regulating the pH value of the concentrated solution-absolute ethyl alcohol mixture obtained in the step (iv) to 3 by using malic acid at 25 ℃, standing for 30 hours at 3 ℃, then centrifuging for 25 minutes at 3 ℃ at 5000rpm, taking the precipitate, and drying the precipitate at 65 ℃ to obtain a rose crude extract;
soaking FL-2 macroporous adsorbent resin in 15 wt.% ethanol water solution at 25 deg.C for 15h, washing the resin with 15 wt.% ethanol water solution until the ethanol eluate is mixed with water and there is no white turbidity, and packing the washed resin into column according to the ratio of resin diameter to column height of 1: 9;
seventhly, mixing the rose crude extract obtained in the fifth step with 80 wt.% aqueous solution of ethanol according to the mass ratio of 1:1000, and stirring at the rotating speed of 300rpm for 20min to obtain the rose crude extract-aqueous solution of ethanol;
eighthly, loading the rose crude extract-ethanol aqueous solution obtained in the step (seventhly) at 25 ℃, wherein the loading amount is 15 percent of the weight of the resin, the loading flow rate is 0.85mL/min, and the standing time is 25 min; then, washing with distilled water and 75 wt.% ethanol water solution to remove impurities; the mass ratio of the distilled water to the resin is 5: 1; the mass ratio of the ethanol aqueous solution with the concentration of 75 wt.% to the resin is 5: 1; the washing flow rate is 30mL/min, the elution flow rate is 38mL/min, and high-purity eluent is collected;
ninthly, freeze-drying the high-purity eluent obtained in the step (b) at the temperature of 50 ℃ below zero and under the air pressure of 10kPa until powder solid is obtained, namely the rose extract.
The preparation method of the rose whitening essence comprises the following steps: mixing the deionized water, the cosolvent, the whitening agent, the softening agent, the emulsifier, the pH regulator and the preservative, and homogenizing at the rotating speed of 15000rpm at 20 ℃ for 3min to obtain a mixed solution; the concentrations of the cosolvent, the whitening agent, the emollient, the emulsifier, the pH regulator and the preservative are 33.2 wt.%, 11.3 wt.%, 1.7 wt.%, 1.2 wt.%, 0.7 wt.% and 0.5 wt.%, respectively, and the balance is deionized water; and mixing the mixed solution and the thickening agent according to a mass ratio of 96.8:3.2, and homogenizing at the rotating speed of 15000rpm at 20 ℃ for 3min to obtain the rose whitening essence.
Example 3
A rose whitening essence comprises deionized water, cosolvent, thickener, whitening agent, emollient, emulsifier, pH regulator, and antiseptic.
The preparation method of the cosolvent comprises the following steps: mixing absolute ethyl alcohol, glycerol, propylene carbonate and 1, 3-butanediol according to the mass ratio of 27.2:13.1:7.6:5.8 at 20 ℃, and carrying out homogenization treatment at the rotating speed of 15000rpm for 2min to obtain the cosolvent.
The preparation method of the thickening agent comprises the following steps: mixing trehalose, betaine, linoleic acid and absolute ethyl alcohol according to the mass ratio of 11.7:5.3:3.8:18.1 at 20 ℃, and stirring at the rotating speed of 1200rpm for 15min to obtain the thickening agent.
The preparation method of the whitening agent comprises the following steps: mixing the rose extract, the iris tonkinensis root extract, the sage extract, the Sudan cola nut extract and the 1, 3-butanediol according to the mass ratio of 67.3:16.3:15.7:7.1:201.2 at 20 ℃, and homogenizing at the rotating speed of 15000rpm for 2min to obtain the whitening agent.
The preparation method of the softening agent comprises the following steps: mixing the cyclohexasiloxane, the polydimethylsiloxane, the squalane and the 1, 3-butanediol according to the mass ratio of 19.1:13.5:9.8:68.6 at 20 ℃, and homogenizing at the rotating speed of 15000rpm for 2min to obtain the softening agent.
The preparation method of the emulsifier comprises the following steps: isocetyl polyether-10, PPG-6-decyltetradecyl polyether-20 and absolute ethyl alcohol were mixed at a mass ratio of 13.8:4.7:43.2 at 20 ℃ and homogenized at 15000rpm for 2min to obtain the emulsifier.
The preparation method of the pH regulator comprises the following steps: and mixing dipotassium phosphate, sodium bicarbonate, potassium hydroxide and deionized water according to the mass ratio of 9.1:3.3:2.7:31.9 at 20 ℃, and stirring at the rotating speed of 1200rpm for 10min to obtain the pH regulator.
The preparation method of the preservative comprises the following steps: mixing potassium sorbate, sodium metabisulfite and deionized water according to the mass ratio of 1.7:1.2:10.3, and stirring at the rotating speed of 1200rpm for 8min to obtain the preservative.
The preparation method of the rose extract comprises the following steps:
firstly, rose petals, 75 wt.% ethanol water solution and a penetration enhancer are mixed according to the mass ratio of 5:5:1 at 25 ℃, stirred for 20 hours at the rotating speed of 300rpm, and simultaneously treated by ultrasonic waves with the power of 400w and the frequency of 42kHz to obtain rose soaking substances; the penetration enhancer is lemongrass oil;
secondly, carrying out pressure filtration on the rose soaked substance obtained in the first step for 45min by adopting the pressure of 1MPa to obtain a filtrate, centrifuging the filtrate for 25min at the rotating speed of 5000rpm, and collecting a supernatant;
thirdly, concentrating the supernatant obtained in the second step to 50 percent of the volume of the original supernatant under the conditions of-50 ℃ and 10kPa to obtain concentrated solution;
fourthly, mixing the concentrated solution obtained in the third step with absolute ethyl alcohol at 25 ℃, stirring for 40min at the rotating speed of 300rpm, and simultaneously treating with ultrasonic waves with the power of 400w and the frequency of 42kHz to obtain a concentrated solution-absolute ethyl alcohol mixture; the concentration of absolute ethanol in the concentrate-absolute ethanol mixture was 80 wt.%;
fifthly, regulating the pH value of the concentrated solution-absolute ethyl alcohol mixture obtained in the step (iv) to 3 by using malic acid at 25 ℃, standing for 30 hours at 3 ℃, then centrifuging for 25 minutes at 3 ℃ at 5000rpm, taking the precipitate, and drying the precipitate at 65 ℃ to obtain a rose crude extract;
soaking FL-2 macroporous adsorbent resin in 15 wt.% ethanol water solution at 25 deg.C for 15h, washing the resin with 15 wt.% ethanol water solution until the ethanol eluate is mixed with water and there is no white turbidity, and packing the washed resin into column according to the ratio of resin diameter to column height of 1: 9;
seventhly, mixing the rose crude extract obtained in the fifth step with 80 wt.% aqueous solution of ethanol according to the mass ratio of 1:1000, and stirring at the rotating speed of 300rpm for 20min to obtain the rose crude extract-aqueous solution of ethanol;
eighthly, loading the rose crude extract-ethanol aqueous solution obtained in the step (seventhly) at 25 ℃, wherein the loading amount is 15 percent of the weight of the resin, the loading flow rate is 0.85mL/min, and the standing time is 25 min; then, washing with distilled water and 75 wt.% ethanol water solution to remove impurities; the mass ratio of the distilled water to the resin is 5: 1; the mass ratio of the ethanol aqueous solution with the concentration of 75 wt.% to the resin is 5: 1; the washing flow rate is 30mL/min, the elution flow rate is 38mL/min, and high-purity eluent is collected;
ninthly, freeze-drying the high-purity eluent obtained in the step (b) at the temperature of 50 ℃ below zero and under the air pressure of 10kPa until powder solid is obtained, namely the rose extract.
The preparation method of the rose whitening essence comprises the following steps: mixing the deionized water, the cosolvent, the whitening agent, the softening agent, the emulsifier, the pH regulator and the preservative, and homogenizing at the rotating speed of 15000rpm at 20 ℃ for 3min to obtain a mixed solution; the concentrations of the cosolvent, the whitening agent, the emollient, the emulsifier, the pH regulator and the preservative are 33.2 wt.%, 11.3 wt.%, 1.7 wt.%, 1.2 wt.%, 0.7 wt.% and 0.5 wt.%, respectively, and the balance is deionized water; and mixing the mixed solution and the thickening agent according to a mass ratio of 96.8:3.2, and homogenizing at the rotating speed of 15000rpm at 20 ℃ for 3min to obtain the rose whitening essence.
Comparative example 1
A rose whitening essence comprises deionized water, cosolvent, thickener, whitening agent, emollient, emulsifier, pH regulator, and antiseptic.
The preparation method of the cosolvent comprises the following steps: mixing absolute ethyl alcohol, glycerol, propylene carbonate and 1, 3-butanediol according to the mass ratio of 27.2:13.1:7.6:5.8 at 20 ℃, and carrying out homogenization treatment at the rotating speed of 15000rpm for 2min to obtain the cosolvent.
The preparation method of the thickening agent comprises the following steps: mixing trehalose, betaine, linoleic acid and absolute ethyl alcohol according to the mass ratio of 11.7:5.3:3.8:18.1 at 20 ℃, and stirring at the rotating speed of 1200rpm for 15min to obtain the thickening agent.
The preparation method of the whitening agent comprises the following steps: mixing the rose extract, the iris tonkinensis root extract, the sage extract, the Sudan cola nut extract and the 1, 3-butanediol according to the mass ratio of 67.3:16.3:15.7:7.1:201.2 at 20 ℃, and homogenizing at the rotating speed of 15000rpm for 2min to obtain the whitening agent.
The preparation method of the softening agent comprises the following steps: mixing the cyclohexasiloxane, the polydimethylsiloxane, the squalane and the 1, 3-butanediol according to the mass ratio of 19.1:13.5:9.8:68.6 at 20 ℃, and homogenizing at the rotating speed of 15000rpm for 2min to obtain the softening agent.
The preparation method of the emulsifier comprises the following steps: isocetyl polyether-10, PPG-6-decyltetradecyl polyether-20 and absolute ethyl alcohol were mixed at a mass ratio of 13.8:4.7:43.2 at 20 ℃ and homogenized at 15000rpm for 2min to obtain the emulsifier.
The preparation method of the pH regulator comprises the following steps: and mixing dipotassium phosphate, sodium bicarbonate, potassium hydroxide and deionized water according to the mass ratio of 9.1:3.3:2.7:31.9 at 20 ℃, and stirring at the rotating speed of 1200rpm for 10min to obtain the pH regulator.
The preparation method of the preservative comprises the following steps: mixing potassium sorbate, sodium metabisulfite and deionized water according to the mass ratio of 1.7:1.2:10.3, and stirring at the rotating speed of 1200rpm for 8min to obtain the preservative.
The preparation method of the rose extract comprises the following steps:
firstly, rose petals, 75 wt.% ethanol water solution and a penetration enhancer are mixed according to the mass ratio of 5:5:1 at 25 ℃, stirred for 20 hours at the rotating speed of 300rpm, and simultaneously treated by ultrasonic waves with the power of 400w and the frequency of 42kHz to obtain rose soaking substances; the penetration enhancer is peppermint oil;
secondly, carrying out pressure filtration on the rose soaked substance obtained in the first step for 45min by adopting the pressure of 1MPa to obtain a filtrate, centrifuging the filtrate for 25min at the rotating speed of 5000rpm, and collecting a supernatant;
thirdly, concentrating the supernatant obtained in the second step to 50 percent of the volume of the original supernatant under the conditions of-50 ℃ and 10kPa to obtain concentrated solution;
fourthly, mixing the concentrated solution obtained in the third step with absolute ethyl alcohol at 25 ℃, stirring for 40min at the rotating speed of 300rpm, and simultaneously treating with ultrasonic waves with the power of 400w and the frequency of 42kHz to obtain a concentrated solution-absolute ethyl alcohol mixture; the concentration of absolute ethanol in the concentrate-absolute ethanol mixture was 80 wt.%;
fifthly, regulating the pH value of the concentrated solution-absolute ethyl alcohol mixture obtained in the step (iv) to 3 by using malic acid at 25 ℃, standing for 30 hours at 3 ℃, then centrifuging for 25 minutes at 3 ℃ at 5000rpm, taking the precipitate, and drying the precipitate at 65 ℃ to obtain a rose crude extract;
soaking FL-2 macroporous adsorbent resin in 15 wt.% ethanol water solution at 25 deg.C for 15h, washing the resin with 15 wt.% ethanol water solution until the ethanol eluate is mixed with water and there is no white turbidity, and packing the washed resin into column according to the ratio of resin diameter to column height of 1: 9;
seventhly, mixing the rose crude extract obtained in the fifth step with 80 wt.% aqueous solution of ethanol according to the mass ratio of 1:1000, and stirring at the rotating speed of 300rpm for 20min to obtain the rose crude extract-aqueous solution of ethanol;
eighthly, loading the rose crude extract-ethanol aqueous solution obtained in the step (seventhly) at 25 ℃, wherein the loading amount is 15 percent of the weight of the resin, the loading flow rate is 0.85mL/min, and the standing time is 25 min; then, washing with distilled water and 75 wt.% ethanol water solution to remove impurities; the mass ratio of the distilled water to the resin is 5: 1; the mass ratio of the ethanol aqueous solution with the concentration of 75 wt.% to the resin is 5: 1; the washing flow rate is 30mL/min, the elution flow rate is 38mL/min, and high-purity eluent is collected;
ninthly, freeze-drying the high-purity eluent obtained in the step (b) at the temperature of 50 ℃ below zero and under the air pressure of 10kPa until powder solid is obtained, namely the rose extract.
The preparation method of the rose whitening essence comprises the following steps: mixing the deionized water, the cosolvent, the whitening agent, the softening agent, the emulsifier, the pH regulator and the preservative, and homogenizing at the rotating speed of 15000rpm at 20 ℃ for 3min to obtain a mixed solution; the concentrations of the cosolvent, the whitening agent, the emollient, the emulsifier, the pH regulator and the preservative are 33.2 wt.%, 11.3 wt.%, 1.7 wt.%, 1.2 wt.%, 0.7 wt.% and 0.5 wt.%, respectively, and the balance is deionized water; and mixing the mixed solution and the thickening agent according to a mass ratio of 96.8:3.2, and homogenizing at the rotating speed of 15000rpm at 20 ℃ for 3min to obtain the rose whitening essence.
Comparative example 2
A rose whitening essence comprises deionized water, cosolvent, thickener, whitening agent, emollient, emulsifier, pH regulator, and antiseptic.
The preparation method of the cosolvent comprises the following steps: mixing absolute ethyl alcohol, glycerol, propylene carbonate and 1, 3-butanediol according to the mass ratio of 27.2:13.1:7.6:5.8 at 20 ℃, and carrying out homogenization treatment at the rotating speed of 15000rpm for 2min to obtain the cosolvent.
The preparation method of the thickening agent comprises the following steps: mixing trehalose, betaine, linoleic acid and absolute ethyl alcohol according to the mass ratio of 11.7:5.3:3.8:18.1 at 20 ℃, and stirring at the rotating speed of 1200rpm for 15min to obtain the thickening agent.
The preparation method of the whitening agent comprises the following steps: mixing the rose extract, the iris tonkinensis root extract, the sage extract, the Sudan cola nut extract and the 1, 3-butanediol according to the mass ratio of 67.3:16.3:15.7:7.1:201.2 at 20 ℃, and homogenizing at the rotating speed of 15000rpm for 2min to obtain the whitening agent.
The preparation method of the softening agent comprises the following steps: mixing the cyclohexasiloxane, the polydimethylsiloxane, the squalane and the 1, 3-butanediol according to the mass ratio of 19.1:13.5:9.8:68.6 at 20 ℃, and homogenizing at the rotating speed of 15000rpm for 2min to obtain the softening agent.
The preparation method of the emulsifier comprises the following steps: isocetyl polyether-10, PPG-6-decyltetradecyl polyether-20 and absolute ethyl alcohol were mixed at a mass ratio of 13.8:4.7:43.2 at 20 ℃ and homogenized at 15000rpm for 2min to obtain the emulsifier.
The preparation method of the pH regulator comprises the following steps: and mixing dipotassium phosphate, sodium bicarbonate, potassium hydroxide and deionized water according to the mass ratio of 9.1:3.3:2.7:31.9 at 20 ℃, and stirring at the rotating speed of 1200rpm for 10min to obtain the pH regulator.
The preparation method of the preservative comprises the following steps: mixing potassium sorbate, sodium metabisulfite and deionized water according to the mass ratio of 1.7:1.2:10.3, and stirring at the rotating speed of 1200rpm for 8min to obtain the preservative.
The preparation method of the rose extract comprises the following steps:
firstly, rose petals, 75 wt.% ethanol water solution and a penetration enhancer are mixed according to the mass ratio of 5:5:1 at 25 ℃, stirred for 20 hours at the rotating speed of 300rpm, and simultaneously treated by ultrasonic waves with the power of 400w and the frequency of 42kHz to obtain rose soaking substances; the penetration enhancer is a mixture of litsea cubeba oil and peppermint oil according to the mass ratio of 1: 1;
secondly, carrying out pressure filtration on the rose soaked substance obtained in the first step for 45min by adopting the pressure of 1MPa to obtain a filtrate, centrifuging the filtrate for 25min at the rotating speed of 5000rpm, and collecting a supernatant;
thirdly, concentrating the supernatant obtained in the second step to 50 percent of the volume of the original supernatant under the conditions of-50 ℃ and 10kPa to obtain concentrated solution;
fourthly, mixing the concentrated solution obtained in the third step with absolute ethyl alcohol at 25 ℃, stirring for 40min at the rotating speed of 300rpm, and simultaneously treating with ultrasonic waves with the power of 400w and the frequency of 42kHz to obtain a concentrated solution-absolute ethyl alcohol mixture; the concentration of absolute ethanol in the concentrate-absolute ethanol mixture was 80 wt.%;
fifthly, regulating the pH value of the concentrated solution-absolute ethyl alcohol mixture obtained in the step (iv) to 3 by using malic acid at 25 ℃, standing for 30 hours at 3 ℃, then centrifuging for 25 minutes at 3 ℃ at 5000rpm, taking the precipitate, and drying the precipitate at 65 ℃ to obtain a rose crude extract;
soaking FL-2 macroporous adsorbent resin in 15 wt.% ethanol water solution at 25 deg.C for 15h, washing the resin with 15 wt.% ethanol water solution until the ethanol eluate is mixed with water and there is no white turbidity, and packing the washed resin into column according to the ratio of resin diameter to column height of 1: 9;
seventhly, mixing the rose crude extract obtained in the fifth step with 80 wt.% aqueous solution of ethanol according to the mass ratio of 1:1000, and stirring at the rotating speed of 300rpm for 20min to obtain the rose crude extract-aqueous solution of ethanol;
eighthly, loading the rose crude extract-ethanol aqueous solution obtained in the step (seventhly) at 25 ℃, wherein the loading amount is 15 percent of the weight of the resin, the loading flow rate is 0.85mL/min, and the standing time is 25 min; then, washing with distilled water and 75 wt.% ethanol water solution to remove impurities; the mass ratio of the distilled water to the resin is 5: 1; the mass ratio of the ethanol aqueous solution with the concentration of 75 wt.% to the resin is 5: 1; the washing flow rate is 30mL/min, the elution flow rate is 38mL/min, and high-purity eluent is collected;
ninthly, freeze-drying the high-purity eluent obtained in the step (b) at the temperature of 50 ℃ below zero and under the air pressure of 10kPa until powder solid is obtained, namely the rose extract.
The preparation method of the rose whitening essence comprises the following steps: mixing the deionized water, the cosolvent, the whitening agent, the softening agent, the emulsifier, the pH regulator and the preservative, and homogenizing at the rotating speed of 15000rpm at 20 ℃ for 3min to obtain a mixed solution; the concentrations of the cosolvent, the whitening agent, the emollient, the emulsifier, the pH regulator and the preservative are 33.2 wt.%, 11.3 wt.%, 1.7 wt.%, 1.2 wt.%, 0.7 wt.% and 0.5 wt.%, respectively, and the balance is deionized water; and mixing the mixed solution and the thickening agent according to a mass ratio of 96.8:3.2, and homogenizing at the rotating speed of 15000rpm at 20 ℃ for 3min to obtain the rose whitening essence.
Comparative example 3
A rose whitening essence comprises deionized water, cosolvent, thickener, whitening agent, emollient, emulsifier, pH regulator, and antiseptic.
The preparation method of the cosolvent comprises the following steps: mixing absolute ethyl alcohol, glycerol, propylene carbonate and 1, 3-butanediol according to the mass ratio of 27.2:13.1:7.6:5.8 at 20 ℃, and carrying out homogenization treatment at the rotating speed of 15000rpm for 2min to obtain the cosolvent.
The preparation method of the thickening agent comprises the following steps: mixing trehalose, betaine, linoleic acid and absolute ethyl alcohol according to the mass ratio of 11.7:5.3:3.8:18.1 at 20 ℃, and stirring at the rotating speed of 1200rpm for 15min to obtain the thickening agent.
The preparation method of the whitening agent comprises the following steps: mixing the rose extract, the iris tonkinensis root extract, the sage extract, the Sudan cola nut extract and the 1, 3-butanediol according to the mass ratio of 67.3:16.3:15.7:7.1:201.2 at 20 ℃, and homogenizing at the rotating speed of 15000rpm for 2min to obtain the whitening agent.
The preparation method of the softening agent comprises the following steps: mixing the cyclohexasiloxane, the polydimethylsiloxane, the squalane and the 1, 3-butanediol according to the mass ratio of 19.1:13.5:9.8:68.6 at 20 ℃, and homogenizing at the rotating speed of 15000rpm for 2min to obtain the softening agent.
The preparation method of the emulsifier comprises the following steps: isocetyl polyether-10, PPG-6-decyltetradecyl polyether-20 and absolute ethyl alcohol were mixed at a mass ratio of 13.8:4.7:43.2 at 20 ℃ and homogenized at 15000rpm for 2min to obtain the emulsifier.
The preparation method of the pH regulator comprises the following steps: and mixing dipotassium phosphate, sodium bicarbonate, potassium hydroxide and deionized water according to the mass ratio of 9.1:3.3:2.7:31.9 at 20 ℃, and stirring at the rotating speed of 1200rpm for 10min to obtain the pH regulator.
The preparation method of the preservative comprises the following steps: mixing potassium sorbate, sodium metabisulfite and deionized water according to the mass ratio of 1.7:1.2:10.3, and stirring at the rotating speed of 1200rpm for 8min to obtain the preservative.
The preparation method of the rose extract comprises the following steps:
firstly, rose petals, 75 wt.% ethanol water solution and a penetration enhancer are mixed according to the mass ratio of 5:5:1 at 25 ℃, stirred for 20 hours at the rotating speed of 300rpm, and simultaneously treated by ultrasonic waves with the power of 400w and the frequency of 42kHz to obtain rose soaking substances; the penetration enhancer is a mixture of peppermint oil and lemongrass oil according to the mass ratio of 1: 1;
secondly, carrying out pressure filtration on the rose soaked substance obtained in the first step for 45min by adopting the pressure of 1MPa to obtain a filtrate, centrifuging the filtrate for 25min at the rotating speed of 5000rpm, and collecting a supernatant;
thirdly, concentrating the supernatant obtained in the second step to 50 percent of the volume of the original supernatant under the conditions of-50 ℃ and 10kPa to obtain concentrated solution;
fourthly, mixing the concentrated solution obtained in the third step with absolute ethyl alcohol at 25 ℃, stirring for 40min at the rotating speed of 300rpm, and simultaneously treating with ultrasonic waves with the power of 400w and the frequency of 42kHz to obtain a concentrated solution-absolute ethyl alcohol mixture; the concentration of absolute ethanol in the concentrate-absolute ethanol mixture was 80 wt.%;
fifthly, regulating the pH value of the concentrated solution-absolute ethyl alcohol mixture obtained in the step (iv) to 3 by using malic acid at 25 ℃, standing for 30 hours at 3 ℃, then centrifuging for 25 minutes at 3 ℃ at 5000rpm, taking the precipitate, and drying the precipitate at 65 ℃ to obtain a rose crude extract;
soaking FL-2 macroporous adsorbent resin in 15 wt.% ethanol water solution at 25 deg.C for 15h, washing the resin with 15 wt.% ethanol water solution until the ethanol eluate is mixed with water and there is no white turbidity, and packing the washed resin into column according to the ratio of resin diameter to column height of 1: 9;
seventhly, mixing the rose crude extract obtained in the fifth step with 80 wt.% aqueous solution of ethanol according to the mass ratio of 1:1000, and stirring at the rotating speed of 300rpm for 20min to obtain the rose crude extract-aqueous solution of ethanol;
eighthly, loading the rose crude extract-ethanol aqueous solution obtained in the step (seventhly) at 25 ℃, wherein the loading amount is 15 percent of the weight of the resin, the loading flow rate is 0.85mL/min, and the standing time is 25 min; then, washing with distilled water and 75 wt.% ethanol water solution to remove impurities; the mass ratio of the distilled water to the resin is 5: 1; the mass ratio of the ethanol aqueous solution with the concentration of 75 wt.% to the resin is 5: 1; the washing flow rate is 30mL/min, the elution flow rate is 38mL/min, and high-purity eluent is collected;
ninthly, freeze-drying the high-purity eluent obtained in the step (b) at the temperature of 50 ℃ below zero and under the air pressure of 10kPa until powder solid is obtained, namely the rose extract.
The preparation method of the rose whitening essence comprises the following steps: mixing the deionized water, the cosolvent, the whitening agent, the softening agent, the emulsifier, the pH regulator and the preservative, and homogenizing at the rotating speed of 15000rpm at 20 ℃ for 3min to obtain a mixed solution; the concentrations of the cosolvent, the whitening agent, the emollient, the emulsifier, the pH regulator and the preservative are 33.2 wt.%, 11.3 wt.%, 1.7 wt.%, 1.2 wt.%, 0.7 wt.% and 0.5 wt.%, respectively, and the balance is deionized water; and mixing the mixed solution and the thickening agent according to a mass ratio of 96.8:3.2, and homogenizing at the rotating speed of 15000rpm at 20 ℃ for 3min to obtain the rose whitening essence.
Comparative example 4
A rose whitening essence comprises deionized water, cosolvent, thickener, whitening agent, emollient, emulsifier, pH regulator, and antiseptic.
The preparation method of the cosolvent comprises the following steps: mixing absolute ethyl alcohol, glycerol, propylene carbonate and 1, 3-butanediol according to the mass ratio of 27.2:13.1:7.6:5.8 at 20 ℃, and carrying out homogenization treatment at the rotating speed of 15000rpm for 2min to obtain the cosolvent.
The preparation method of the thickening agent comprises the following steps: mixing trehalose, betaine, linoleic acid and absolute ethyl alcohol according to the mass ratio of 11.7:5.3:3.8:18.1 at 20 ℃, and stirring at the rotating speed of 1200rpm for 15min to obtain the thickening agent.
The preparation method of the whitening agent comprises the following steps: mixing the rose extract, the iris tonkinensis root extract, the sage extract, the Sudan cola nut extract and the 1, 3-butanediol according to the mass ratio of 67.3:16.3:15.7:7.1:201.2 at 20 ℃, and homogenizing at the rotating speed of 15000rpm for 2min to obtain the whitening agent.
The preparation method of the softening agent comprises the following steps: mixing the cyclohexasiloxane, the polydimethylsiloxane, the squalane and the 1, 3-butanediol according to the mass ratio of 19.1:13.5:9.8:68.6 at 20 ℃, and homogenizing at the rotating speed of 15000rpm for 2min to obtain the softening agent.
The preparation method of the emulsifier comprises the following steps: isocetyl polyether-10, PPG-6-decyltetradecyl polyether-20 and absolute ethyl alcohol were mixed at a mass ratio of 13.8:4.7:43.2 at 20 ℃ and homogenized at 15000rpm for 2min to obtain the emulsifier.
The preparation method of the pH regulator comprises the following steps: and mixing dipotassium phosphate, sodium bicarbonate, potassium hydroxide and deionized water according to the mass ratio of 9.1:3.3:2.7:31.9 at 20 ℃, and stirring at the rotating speed of 1200rpm for 10min to obtain the pH regulator.
The preparation method of the preservative comprises the following steps: mixing potassium sorbate, sodium metabisulfite and deionized water according to the mass ratio of 1.7:1.2:10.3, and stirring at the rotating speed of 1200rpm for 8min to obtain the preservative.
The preparation method of the rose extract comprises the following steps:
firstly, rose petals and 75 wt.% ethanol water solution are mixed according to the mass ratio of 1:1 at 25 ℃, stirred for 20 hours at the rotating speed of 300rpm, and simultaneously treated by ultrasonic waves with the power of 400w and the frequency of 42kHz to obtain rose soaking matter;
secondly, carrying out pressure filtration on the rose soaked substance obtained in the first step for 45min by adopting the pressure of 1MPa to obtain a filtrate, centrifuging the filtrate for 25min at the rotating speed of 5000rpm, and collecting a supernatant;
thirdly, concentrating the supernatant obtained in the second step to 50 percent of the volume of the original supernatant under the conditions of-50 ℃ and 10kPa to obtain concentrated solution;
fourthly, mixing the concentrated solution obtained in the third step with absolute ethyl alcohol at 25 ℃, stirring for 40min at the rotating speed of 300rpm, and simultaneously treating with ultrasonic waves with the power of 400w and the frequency of 42kHz to obtain a concentrated solution-absolute ethyl alcohol mixture; the concentration of absolute ethanol in the concentrate-absolute ethanol mixture was 80 wt.%;
fifthly, regulating the pH value of the concentrated solution-absolute ethyl alcohol mixture obtained in the step (iv) to 3 by using malic acid at 25 ℃, standing for 30 hours at 3 ℃, then centrifuging for 25 minutes at 3 ℃ at 5000rpm, taking the precipitate, and drying the precipitate at 65 ℃ to obtain a rose crude extract;
soaking FL-2 macroporous adsorbent resin in 15 wt.% ethanol water solution at 25 deg.C for 15h, washing the resin with 15 wt.% ethanol water solution until the ethanol eluate is mixed with water and there is no white turbidity, and packing the washed resin into column according to the ratio of resin diameter to column height of 1: 9;
seventhly, mixing the rose crude extract obtained in the fifth step with 80 wt.% aqueous solution of ethanol according to the mass ratio of 1:1000, and stirring at the rotating speed of 300rpm for 20min to obtain the rose crude extract-aqueous solution of ethanol;
eighthly, loading the rose crude extract-ethanol aqueous solution obtained in the step (seventhly) at 25 ℃, wherein the loading amount is 15 percent of the weight of the resin, the loading flow rate is 0.85mL/min, and the standing time is 25 min; then, washing with distilled water and 75 wt.% ethanol water solution to remove impurities; the mass ratio of the distilled water to the resin is 5: 1; the mass ratio of the ethanol aqueous solution with the concentration of 75 wt.% to the resin is 5: 1; the washing flow rate is 30mL/min, the elution flow rate is 38mL/min, and high-purity eluent is collected;
ninthly, freeze-drying the high-purity eluent obtained in the step (b) at the temperature of 50 ℃ below zero and under the air pressure of 10kPa until powder solid is obtained, namely the rose extract.
The preparation method of the rose whitening essence comprises the following steps: mixing the deionized water, the cosolvent, the whitening agent, the softening agent, the emulsifier, the pH regulator and the preservative, and homogenizing at the rotating speed of 15000rpm at 20 ℃ for 3min to obtain a mixed solution; the concentrations of the cosolvent, the whitening agent, the emollient, the emulsifier, the pH regulator and the preservative are 33.2 wt.%, 11.3 wt.%, 1.7 wt.%, 1.2 wt.%, 0.7 wt.% and 0.5 wt.%, respectively, and the balance is deionized water; and mixing the mixed solution and the thickening agent according to a mass ratio of 96.8:3.2, and homogenizing at the rotating speed of 15000rpm at 20 ℃ for 3min to obtain the rose whitening essence.
Test example 1
And (3) testing the whitening effect: 112 subjects were selected, aged between 22 and 35 years, and all subjects were divided into 7 comparison groups, each consisting of half a total of 16 persons each. The rose whitening liquid prepared in examples 1 to 3 and comparative examples 1 to 4 was used by each comparative group for a total test period of 28 days, 3 times per day, and was applied to both cheeks uniformly after cleansing, in an amount of 1mL each time. No other whitening products were used during the test. The skin was tested for its haematochrome content and its lightness (L value) using a multi-probe skin tester (MPA10, from CK company, germany) before (0d), on day 14 (14d) and on day 28 (28 d). The two indexes are the average value of the test results in each comparison group. The test results are shown in tables 1 and 2.
TABLE 1 Red pigment content of skin before and after use of the rose whitening liquid obtained in each example of the present invention and comparative example
TABLE 2 skin Brightness before and after use of the rose whitening liquid obtained in each example of the present invention and comparative example
Test example 2
And (3) testing the flavone content: according to Al (NO)3)3Color development with rutinMeasuring the absorbance value of the gradient concentration solution of the standard substance; the regression equation of the solution concentration (c) versus absorbance (A) curve is: c 10.24A +0.012, R20.9993. The rose extracts obtained in the embodiments and the comparative examples of the invention are diluted to proper concentrations, the flavone content in the rose extracts obtained in the embodiments is measured, the mass concentration of the diluted flavone extracting solution is obtained according to the regression equation, the mass concentration of the original rose extract is obtained according to the dilution times, and finally the mass concentration of the total flavone in the rose is calculated. The test results are shown in table 3.
TABLE 3 flavone content in rose extracts obtained from the examples of the present invention and the comparative examples
Test example 3
Free radical scavenging ability test: preparing a DPPH free radical standard solution: weighing 0.0256g of DPPH free radical reagent, and preparing a DPPH free radical standard solution with the mass concentration of 0.0256g/L by taking absolute ethyl alcohol as a solvent; respectively sucking 1.0, 2.0, 3.0, 4.0, 5.0, 6.0, 7.0, 8.0, 9.0 and 10.0mL of the DPPH free radical standard solution in a test tube, wherein less than 10mL of the DPPH free radical standard solution is supplemented by absolute ethyl alcohol; thirdly, determining the absorbance of each solution at the wavelength of 517nm by taking absolute ethyl alcohol as a blank, and obtaining a regression equation of the relation curve of the absorbance and the mass concentration of the DPPH free radical solution: y is 0.0259x +0.0018(R2 is 0.9996), and the relation curve shows that the mass concentration and the absorbance of the DPPH free radical solution have a strong linear relation in the range of 2.56-25.60 mg/L, which shows that the absorbance of the DPPH free radical solution in the range can be used as an index for measuring the amount concentration of DPPH free matrix in the solution; fourth, absolute ethyl alcohol is used as a solvent, and rose extracts with mass concentrations of 0.004, 0.012, 0.016, 0.024, 0.050, 0.100, 0.150mg/mL and 0.300mg/mL obtained in each example of the invention and each comparative example are prepared as solutions to be tested; fifthly, absorbing 5mL of the solution to be detected, adding 5mL of the DPPH free radical standard solution, uniformly mixing, reacting for 30min, and measuring absorbance; sixthly, after the sample to be detected reacts with the DPPH free radical, the residual amount of the DPPH free radical can be obtained according to the following formula: residual DPPH radical,/% (DPPH radical t/DPPH radical 0) × 00, where: DPPH free radical 0 is the initial mass concentration of DPPH free radical; and (3) taking the DPPH free radical t as the mass concentration of DPPH free radicals in a system at the moment t, and subtracting the residual amount of the DPPH free radicals from 100% to obtain the DPPH free radical clearance rate of the rose extract obtained in each example. The test results are shown in table 4.
TABLE 4 DPPH radical scavenging ratio of rose extracts obtained from examples of the present invention and comparative examples
The haematochrome (14d) ═ 58.22E.U., the haematochrome (28d) ═ 52.02E.U., the L value (14d) ═ 59.73, the L value (28d) ═ 65.42, the flavone ═ 728.6mg/g, and the DPPH free radical scavenging rate (96.8%) of example 1 (using litsea cubeba oil or lemongrass oil as the penetration enhancer), comparative examples 1-3 (using peppermint oil and/or litsea cubeba oil and lemongrass oil as the penetration enhancer), comparative example 4 (without the penetration enhancer) the haematochrome (14d) ═ 59.89-68.11E.U., the haematochrome (28d) ═ 52.86-57.99E.U., the L value (14d) ═ 53.40-57.62, L value (28d) ═ 60.51.68, and L value (3519.64.82.0-36709), and the DPPH free radical scavenging rate (96.8%) of example 2-3 (using litsea cubeba oil and lemongrass oil as the penetration enhancer), this is because: the litsea cubeba oil and the lemongrass oil are rich in solvents with active chemical properties, such as alpha-lupinene, alpha-pinene and the like, can effectively promote the rose total flavonoids to seep out of cells of the rose, and improve the collection rate of the filtrate obtained by medium-pressure filtration of the rose soak solution; when the rose extract and the rose flavone are compounded for use, the rose total flavone can be promoted to exude, and simultaneously, the antioxidant protection effect is achieved, and the rose extract with higher rose total flavone content and stronger active ingredient activity can be obtained; the peppermint oil contains more menthol, menthyl acetate and other components, and the effect of improving the collection rate of the total rose flavone obtained from the rose soaked substance is not as good as that of litsea cubeba oil and lemongrass oil. The rose extract contains a large amount of rose total flavonoids which are active ingredients with various beautifying effects of removing free radicals, resisting inflammation, resisting oxidation, removing yellow, brightening, resisting wrinkles, fading spots and the like, can improve the skin state after long-term use, and presents tender, white and bright water. The active ingredients of the vetiver iris root extract, the salvia miltiorrhiza bunge extract, the sudan cola seed extract, the squalane, the trehalose, the linoleic acid, the polydimethylsiloxane and the like can effectively remove free radicals, improve the immunity of the skin, reduce inflammation and sensitivity, reduce the content of red pigment and enable the integral appearance of the skin to be transparent, bright, white and shiny. The active antioxidant components such as total flavonoids in the rose extract prepared by the specific method can promote the metabolism of the generated melanin, has stronger inhibition effect on tyrosinase, simultaneously acts at the source and the route of the melanin, further reduces the content of the melanin in the skin, and further improves the whiteness and the brightness of the skin.
It should be noted that the above embodiments are only used for illustrating the technical solutions of the present invention and are not limited. Although the present invention has been described in detail with reference to the preferred embodiments, it will be understood by those skilled in the art that various changes may be made and equivalents may be substituted without departing from the scope of the present invention.

Claims (7)

1. The rose whitening essence is characterized in that: the whitening and softening agent consists of deionized water, a cosolvent, a thickening agent, a whitening agent, a softening agent, an emulsifier, a pH regulator and a preservative;
the preparation method of the whitening agent comprises the following steps: mixing rose extract, iris tonkinensis root extract, sage herb extract, Sudan cola seed extract and 1, 3-butanediol, and homogenizing to obtain the whitening agent;
the preparation method of the rose extract comprises the following steps:
firstly, rose petals, an ethanol water solution and a penetration enhancer are mixed and stirred, and meanwhile, ultrasonic treatment is carried out to obtain rose soaking matter; the penetration enhancer is one or a mixture of two of litsea cubeba oil and lemongrass oil;
filtering the rose soaked substance obtained in the step I to obtain filtrate, centrifuging the filtrate, and collecting supernatant;
thirdly, concentrating the supernatant obtained in the second step to obtain a concentrated solution;
fourthly, mixing and stirring the concentrated solution obtained in the third step with absolute ethyl alcohol, and simultaneously carrying out ultrasonic treatment to obtain a concentrated solution-absolute ethyl alcohol mixture;
regulating the pH of the concentrated solution-absolute ethyl alcohol mixture obtained in the step (iv) by using malic acid, standing, then performing centrifugal treatment, taking the precipitate, and drying the precipitate to obtain a rose crude extract;
sixthly, soaking FL-2 type macroporous adsorption resin in an ethanol water solution, then washing the resin with the ethanol water solution until no white turbidity exists after the ethanol eluent is mixed with water, and then filling the washed resin into a column;
seventhly, mixing the rose crude extract obtained in the fifth step with an ethanol water solution and stirring to obtain a rose crude extract-ethanol water solution;
eighthly, loading the rose crude extract-ethanol water solution obtained in the step seven; then, washing with distilled water and ethanol water solution successively to remove impurities; collecting high-purity eluent;
ninthly, freeze-drying the high-purity eluent obtained in the step (viii) until powdery solid is obtained, namely the rose extract.
2. The rose whitening essence of claim 1, wherein the cosolvent is prepared by the method comprising the following steps: and mixing absolute ethyl alcohol, glycerol, propylene carbonate and 1, 3-butanediol, and homogenizing to obtain the cosolvent.
3. The rose whitening essence of claim 1, wherein the thickener is prepared by the following steps: mixing trehalose, betaine, linoleic acid and absolute ethyl alcohol, and stirring to obtain the thickening agent.
4. The rose whitening essence of claim 1, wherein the emollient is prepared by the method comprising: mixing and homogenizing cyclohexasiloxane, polydimethylsiloxane, squalane and 1, 3-butanediol to obtain the softening agent.
5. The rose whitening essence of claim 1, wherein the emulsifier is prepared by the following steps: mixing isocetyl polyether-10, PPG-6-decyltetradecyl polyether-20 and anhydrous ethanol, and homogenizing to obtain the emulsifier.
6. The rose whitening essence of claim 1, wherein the pH regulator is prepared by a method comprising: mixing dipotassium hydrogen phosphate, sodium bicarbonate, potassium hydroxide and deionized water and stirring to obtain the pH regulator; the preparation method of the preservative comprises the following steps: and mixing potassium sorbate, sodium metabisulfite and deionized water, and stirring to obtain the preservative.
7. The rose whitening essence according to any one of claims 1 to 6, which is prepared by the following steps: mixing and homogenizing the deionized water, the cosolvent, the whitening agent, the softening agent, the emulsifier, the pH regulator and the preservative to obtain a mixed solution; and mixing the mixed solution and the thickening agent and homogenizing to obtain the rose whitening essence.
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