CN111870571A - Nano plant extract mask and preparation method thereof - Google Patents

Nano plant extract mask and preparation method thereof Download PDF

Info

Publication number
CN111870571A
CN111870571A CN202010825441.0A CN202010825441A CN111870571A CN 111870571 A CN111870571 A CN 111870571A CN 202010825441 A CN202010825441 A CN 202010825441A CN 111870571 A CN111870571 A CN 111870571A
Authority
CN
China
Prior art keywords
nano
plant extract
parts
mass ratio
mask
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Withdrawn
Application number
CN202010825441.0A
Other languages
Chinese (zh)
Inventor
刘婷
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Individual
Original Assignee
Individual
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Individual filed Critical Individual
Priority to CN202010825441.0A priority Critical patent/CN111870571A/en
Publication of CN111870571A publication Critical patent/CN111870571A/en
Withdrawn legal-status Critical Current

Links

Classifications

    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/96Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution
    • A61K8/97Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution from algae, fungi, lichens or plants; from derivatives thereof
    • A61K8/9783Angiosperms [Magnoliophyta]
    • A61K8/9789Magnoliopsida [dicotyledons]
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/19Cosmetics or similar toiletry preparations characterised by the composition containing inorganic ingredients
    • A61K8/29Titanium; Compounds thereof
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/30Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
    • A61K8/33Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing oxygen
    • A61K8/34Alcohols
    • A61K8/345Alcohols containing more than one hydroxy group
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/30Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
    • A61K8/63Steroids; Derivatives thereof
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/92Oils, fats or waxes; Derivatives thereof, e.g. hydrogenation products thereof
    • A61K8/922Oils, fats or waxes; Derivatives thereof, e.g. hydrogenation products thereof of vegetable origin
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/96Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution
    • A61K8/97Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution from algae, fungi, lichens or plants; from derivatives thereof
    • A61K8/9728Fungi, e.g. yeasts
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61QSPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q17/00Barrier preparations; Preparations brought into direct contact with the skin for affording protection against external influences, e.g. sunlight, X-rays or other harmful rays, corrosive materials, bacteria or insect stings
    • A61Q17/04Topical preparations for affording protection against sunlight or other radiation; Topical sun tanning preparations
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61QSPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q19/00Preparations for care of the skin
    • A61Q19/02Preparations 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 TOILETRY PREPARATIONS
    • A61Q19/00Preparations for care of the skin
    • A61Q19/08Anti-ageing preparations
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2800/00Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
    • A61K2800/40Chemical, physico-chemical or functional or structural properties of particular ingredients
    • A61K2800/41Particular ingredients further characterized by their size
    • A61K2800/413Nanosized, i.e. having sizes below 100 nm
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2800/00Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
    • A61K2800/40Chemical, physico-chemical or functional or structural properties of particular ingredients
    • A61K2800/56Compounds, absorbed onto or entrapped into a solid carrier, e.g. encapsulated perfumes, inclusion compounds, sustained release forms
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2800/00Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
    • A61K2800/80Process related aspects concerning the preparation of the cosmetic composition or the storage or application thereof
    • A61K2800/82Preparation or application process involves sonication or ultrasonication
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2800/00Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
    • A61K2800/80Process related aspects concerning the preparation of the cosmetic composition or the storage or application thereof
    • A61K2800/84Products or compounds obtained by lyophilisation, freeze-drying

Landscapes

  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Animal Behavior & Ethology (AREA)
  • General Health & Medical Sciences (AREA)
  • Public Health (AREA)
  • Veterinary Medicine (AREA)
  • Birds (AREA)
  • Epidemiology (AREA)
  • Microbiology (AREA)
  • Dermatology (AREA)
  • Mycology (AREA)
  • Botany (AREA)
  • Engineering & Computer Science (AREA)
  • Biotechnology (AREA)
  • Chemical & Material Sciences (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Emergency Medicine (AREA)
  • Gerontology & Geriatric Medicine (AREA)
  • Inorganic Chemistry (AREA)
  • Cosmetics (AREA)

Abstract

The invention relates to the technical field of cosmetics, in particular to a nano plant extract mask and a preparation method thereof. The nano plant extract mask comprises the following raw materials in parts by weight: glycerol, 1, 3-butanediol, dipotassium glycyrrhizinate, sodium benzoate, water, a nano lipid carrier-plant extract compound and a functionalized titanium oxide compound. According to the invention, the nanometer lipid carrier-plant extract compound is added, so that the effects of anti-inflammation, anti-wrinkle, whitening, moisturizing and the like of the facial mask are improved; the titanium oxide is prepared into the functionalized titanium oxide compound, so that the specific surface area is larger, and the ultraviolet protection function is stronger; further improving the effects of whitening, oxidation resistance, wrinkle resistance and the like of the facial mask. The preparation method of the nano plant extract mask is simple and convenient, and has good application prospect.

Description

Nano plant extract mask and preparation method thereof
Technical Field
The invention relates to the technical field of cosmetics, in particular to a nano plant extract mask and a preparation method thereof.
Background
With the increasing importance of people on skin care, the mask product becomes a common skin care product in life; common facial masks are divided into paste type, tearing type, jelly type, wet tissue type and other forms, and the facial masks isolate external air and pollution by covering the facial masks on the face, improve the skin temperature, expand pores of the skin, promote secretion and metabolism of sweat glands, and facilitate the skin to remove products of epidermal cell metabolism and accumulated grease substances; the active essence components in the facial mask can supplement moisture and nutrients to the skin in time, so that the skin is bright and elastic, and the nourishing effects of moisturizing, whitening, sun screening, antioxidation, wrinkle resistance, aging resistance, inflammation resistance, acne resistance and the like are realized.
The plant extract contains various active ingredients beneficial to skin, has the advantages of green, safety, wide sources and the like, and can be used as a raw material of cosmetics. However, the stability of the general plant active compounds is poor, the absorption rate is low, the bioavailability is not high, and the application of the compounds is greatly limited; therefore, how to improve the utilization rate of plant extracts is an urgent problem to be solved based on natural plant active compounds.
Disclosure of Invention
In view of the above-mentioned drawbacks of the prior art, the technical problems to be solved by the present invention are: aiming at the defects of the prior art, a nano plant extract mask and a preparation method thereof are provided.
In order to achieve the purpose, the invention adopts the technical scheme that:
a nano plant extract mask comprises the following raw materials in parts by weight: 1-10 parts of glycerol, 1-10 parts of 1, 3-butanediol, 0.01-0.2 part of dipotassium glycyrrhizinate, 0.01-0.5 part of sodium benzoate, 95-155 parts of water and 1-10 parts of nano plant extract.
Further, the nano plant extract mask comprises the following raw materials in parts by weight: 1-10 parts of glycerol, 1-10 parts of 1, 3-butanediol, 0.01-0.2 part of dipotassium glycyrrhizinate, 0.01-0.5 part of sodium benzoate, 95-155 parts of water and 1-10 parts of nano lipid carrier-plant extract compound.
The stability of common plant active compounds is poor, the absorption rate is low, and the bioavailability is not high; therefore, the invention adopts the nano lipid carrier-plant extract compound, and the structure of the nano lipid carrier is similar to that of epidermal lipid in skin, so that the biocompatibility is increased, and the transdermal absorption effect of the plant active compound is promoted; meanwhile, the nanometer lipid carrier can further increase the stability of the plant active ingredients, improve the absorption utilization rate and enable the plant active ingredients to be more easily absorbed and utilized.
Further, the nano plant extract mask comprises the following raw materials in parts by weight: 1-10 parts of glycerol, 1-10 parts of 1, 3-butanediol, 0.01-0.2 part of dipotassium glycyrrhizinate, 0.01-0.5 part of sodium benzoate, 95-155 parts of water, 1-10 parts of a nano lipid carrier-plant extract compound and 1-10 parts of a functionalized titanium oxide compound.
According to the invention, the functionalized titanium oxide compound is added into the nano plant extract mask, the specific surface area is larger, and the ultraviolet protection function of the functionalized titanium oxide compound is further enhanced; meanwhile, the thermal stability and the light stability of the functionalized titanium oxide compound are obviously improved, so that the whitening, oxidation resisting and wrinkle resisting effects of the nano plant extract mask are more obvious.
Preferably, the preparation method of the nano lipid carrier-plant extract compound comprises the following steps:
adding lecithin and Tween 20 into deionized water, wherein the mass ratio of the lecithin to the deionized water is (0.5-10): 100-200), the mass ratio of the Tween 20 to the deionized water is (0.5-10): 100-200), stirring for 5-60min at 10-60 ℃, and stirring at the rotating speed of 50-500rpm to obtain an aqueous phase solution A;
uniformly mixing glyceryl monostearate and cetyl palmitate, wherein the mass ratio of the glyceryl monostearate to the cetyl palmitate is (1-10) to (1-20), and heating at 30-100 ℃ for 20-200 min; sequentially adding vegetable oil and nano plant extract, uniformly mixing, wherein the mass ratio of the vegetable oil to the cetyl palmitate is (1-10) to (0.5-5), the mass ratio of the nano plant extract to the cetyl palmitate is (0.1-5) to (0.1-5), and continuously heating at 30-100 ℃ for 10-60min to obtain an oil phase solution B;
adding the water phase solution A into the oil phase solution B, continuously heating at 30-100 deg.C for 10-60min, and stirring at 50-500rpm to obtain mixed phase solution C; homogenizing the mixed phase solution C in a high pressure homogenizer for 5-60min under the homogenizing pressure of 5-60Mpa, and naturally cooling to room temperature; freezing at- (5-30) deg.C for 1-24 hr, lyophilizing in a lyophilizer for 12-96 hr, and setting the temperature at- (5-70) deg.C to obtain the final product;
preferably, the vegetable oil is at least one of rose hip oil, lemon oil and grape seed oil; further preferably, the vegetable oil is a mixture of rose hip oil and lemon oil, and the mass ratio of the rose hip oil to the lemon oil is (0.1-5) to (0.1-5).
Preferably, the preparation method of the nano plant extract comprises the following steps:
crushing the dried plant raw materials by a universal crusher, and sieving by a sieve of 20-200 meshes to obtain plant raw material powder; adding a leaching solution into the plant raw material powder, wherein the mass ratio of the leaching solution to the plant raw material powder is (1-100):1, uniformly mixing, carrying out ultrasonic treatment at 20-100 ℃ for 0.5-5h, wherein the ultrasonic power is 500 plus one hundred thousand (W) and the ultrasonic frequency is 20-100kHz, centrifuging, and filtering to obtain a filtrate;
vacuum concentrating the filtrate in 20-60 deg.C water bath, and drying to obtain plant extract; adding a plant extract into deionized water, wherein the mass ratio of the plant extract to the deionized water is 1 (10-200), ultrasonic dispersion is carried out for 5-60min, the ultrasonic power is 500-1000W, and the ultrasonic frequency is 20-100 kHz; homogenizing in a high pressure homogenizer for 5-60min under 5-60Mpa, and naturally cooling to room temperature; freezing at- (5-30) deg.C for 1-24 hr, lyophilizing in a lyophilizer for 12-96 hr, and setting the temperature at- (5-70) deg.C to obtain the final product;
the leaching liquor is a mixture of ethyl acetate and absolute ethyl alcohol, and the volume ratio of the ethyl acetate to the absolute ethyl alcohol (0.5-10) is 1.
Preferably, the plant material is at least one of carrot, cucumber, agaric, wolfberry fruit and marigold.
Preferably, the nano plant extract is a mixture of a nano carrot extract and a nano marigold extract, and the mass ratio of the nano carrot extract to the nano marigold extract is (0.1-5) to (0.1-5).
Preferably, the preparation method of the titanium oxide microspheres comprises the following steps:
dissolving isopropyl titanate in absolute ethyl alcohol, wherein the mass ratio of the isopropyl titanate to the absolute ethyl alcohol is (0.05-5):1, so as to obtain an isopropyl titanate ethanol solution; dissolving hexadecylamine in absolute ethyl alcohol, wherein the mass ratio of the hexadecylamine to the absolute ethyl alcohol is 1 (50-250), so as to obtain a hexadecylamine ethyl alcohol solution; adding 0.5-2.5 wt% of potassium chloride aqueous solution into the hexadecylamine ethanol solution, wherein the mass ratio of the 0.5-2.5 wt% of potassium chloride aqueous solution to the hexadecylamine ethanol solution is 1 (100- & ltSUB & gt 500- & gt), and uniformly stirring; adding the isopropyl titanate ethanol solution into the hexadecylamine ethanol solution at the speed of 0.1-2mL/min, stirring for 1-20min at the stirring speed of 50-500rpm, wherein the mass ratio of the isopropyl titanate ethanol solution to the hexadecylamine ethanol is 1 (1-30); stopping stirring, and standing at 5-50 deg.C for 3-30 h; filtering, washing with deionized water for three times, and drying.
Preferably, the preparation method of the modified titanium oxide comprises the following steps:
adding the titanium oxide microspheres into deionized water, wherein the mass ratio of the titanium oxide microspheres to the deionized water is 1 (5-50), stirring for 5-60min at 5-50 ℃, and the stirring speed is 50-500 rpm; adding 80-97 wt% of chloroacetic acid at the speed of 0.1-2mL/min, wherein the mass ratio of 80-97 wt% of chloroacetic acid to titanium oxide microspheres is (0.01-2):1, and stirring at the rotating speed of 50-500rpm for 1-10 min; then refluxing for 12-48h at 70-100 ℃, cooling to room temperature, filtering, washing with deionized water for three times, and drying to obtain the product.
Preferably, the preparation method of the surface functionalized titanium oxide comprises the following steps:
dissolving 1, 3-dihydroxyacetone dimer in deionized water, wherein the mass ratio of the 1, 3-dihydroxyacetone dimer to the deionized water is (0.1-5):10, so as to obtain 1, 3-dihydroxyacetone dimer aqueous solution; adding the modified titanium oxide into deionized water, wherein the mass ratio of the modified titanium oxide to the deionized water is 1 (5-50), and stirring for 1-60min at 5-50 ℃; then 80-98 wt% of sulfuric acid is added, and the mass ratio of the 80-98 wt% of sulfuric acid to the modified titanium oxide is (0.01-1) to (0.1-10); adding 1, 3-dihydroxyacetone dimer aqueous solution, wherein the mass ratio of the 1, 3-dihydroxyacetone dimer aqueous solution to the modified titanium oxide is (5-20):1, stirring for 1-5h at the temperature of 60-100 ℃, and the stirring speed is 50-500 rpm; cooling to room temperature, filtering, washing with deionized water for three times, and drying.
Preferably, the preparation method of the functionalized titanium oxide compound comprises the following steps:
adding the surface functionalized titanium oxide into deionized water, wherein the mass ratio of the surface functionalized titanium oxide to the deionized water is 1 (1-50), and stirring for 5-60min at 5-50 ℃; adding arginine, uniformly mixing, stirring at 50-100 ℃ for 1-10h and 50-500rpm, cooling to room temperature, filtering, washing with deionized water for three times, and drying to obtain the surface functionalized titanium oxide.
The invention also discloses a preparation method of the nano plant extract mask, which comprises the following steps: mixing the raw materials uniformly according to the formula, stirring for 5-60min at 20-60 ℃, and stirring speed of 50-500 rpm; homogenizing in a high pressure homogenizer for 5-60min under 5-60 Mpa; naturally cooling to room temperature, inspecting, filling into facial mask bags containing facial mask carrier, filling 1-20g each bag, vacuum drying in microwave vacuum drier for 0.5-5 hr, and vacuum sealing.
The nanometer plant extract facial mask adopts nanometer plant extract, improves the stability and absorptivity of plant active ingredients, and has better bioavailability. The prepared nano lipid carrier-plant extract compound is used for the nano plant extract mask, so that the effects of resisting inflammation, resisting wrinkles, whitening, moisturizing and the like of the mask are obviously improved; the structure of the nano lipid carrier is similar to that of epidermal lipid in skin, so that the biocompatibility is increased, the nano lipid carrier is used as a carrier of a transdermal active ingredient, the transdermal absorption of a plant active compound is promoted, and meanwhile, the contact surface with skin cells is increased, so that the plant active ingredient is released more quickly and stably and is absorbed by the skin; in addition, the structure of the nano lipid carrier also increases the stability of the active ingredients of the plants and improves the absorption utilization rate; adding a functionalized titanium oxide compound into a nano plant extract mask; compared with titanium oxide, the functionalized titanium oxide compound has larger specific surface area, enhanced ultraviolet protection function and obviously improved thermal stability and light stability; further improving the effects of whitening, oxidation resistance, wrinkle resistance and the like of the facial mask.
The invention has the advantages of
The nanometer plant extract facial mask prepared by adding the nanometer plant extract is more green and safe; the nanometer plant extract is further prepared into a nanometer lipid carrier-plant extract compound, so that the biocompatibility of the nanometer plant extract and the contact surface of the nanometer plant extract and skin cells are increased, the active ingredients of the plant are released more quickly and stably and are absorbed by the skin, and the effects of anti-inflammation, anti-wrinkle, whitening, moisturizing and the like of the mask are improved; the titanium oxide is prepared into the functionalized titanium oxide compound, so that the functionalized titanium oxide compound has larger specific surface area, stronger ultraviolet protection function and better thermal stability and light stability; further improving the effects of whitening, oxidation resistance, wrinkle resistance and the like of the facial mask. The preparation method of the nano plant extract mask is simple and convenient, and has good application prospect.
Detailed Description
Some of the raw materials in the examples and comparative examples are as follows:
cetyl palmitate in examples and comparative examples: CAS number: 540-10-3; shopping in ladder loving (Shanghai)
And (4) chemical industry.
Examples and comparative examples glyceryl monostearate: CAS number: 31566-31-1; purchased from Tianjin Xianshi Biochemical.
Tween 20 in examples and comparative examples: CAS number: 9005-64-5; purchased from shanghai jen chemical.
Lecithin in examples and comparative examples: CAS number: 8002-43-5; soybean is taken as a source; product numbering: m27072; purchased from maire chemical in shanghai.
Lemon oil in examples and comparative examples: CAS number: 8008-56-8; bought from Jiangxi Baolin natural perfume.
Rose hip oil in examples and comparative examples: CAS number: 84603-93-0; purchased from Jiangxi Baicao pharmaceutical industry.
Isopropyl titanate in examples and comparative examples: CAS number: 546-68-9; purchased from Shanghai Aladdin.
Hexadecylamine in examples and comparative examples: CAS number: 143-27-1; purchased from michelin, shanghai.
1, 3-dihydroxyacetone dimer in examples and comparative examples: CAS number: 62147-49-3; purchased from alfa aesar (china).
Lemon oil in examples and comparative examples: CAS number: 8008-56-8; bought from Jiangxi Baolin natural perfume.
In the examples and comparative examples, carrot was selected as the root and the origin was Changzhou, Jiangsu.
In the examples and comparative examples, flos Chrysanthemi is selected, and Yunan Jing is the producing area.
The universal pulverizer used in the examples and comparative examples was a 130B model universal pulverizer available from Tanzhou King Cheng pharmaceutical machinery, Inc., and the main shaft rotation speed was 7000 r/min.
In the examples and comparative examples, a high-pressure homogenizer model SPY-60, manufactured by shanghai shun instrument experimental facilities ltd, was used, and the rated pressure: 0-60 MPa.
Examples and comparative examples a freeze dryer was used, model LGJ-10N bench freeze dryer, vacuum: <10 pa; the total power 950W.
Comparative example 1
The mask comprises the following raw materials in parts by weight: 8 parts of glycerol, 7 parts of 1, 3-butanediol, 0.05 part of dipotassium glycyrrhizinate, 0.18 part of sodium benzoate and 105 parts of water;
the preparation method of the facial mask comprises the following steps: uniformly mixing the raw materials according to a formula, stirring for 30min at 50 ℃, and stirring rotating speed of 300 rpm; homogenizing in a high pressure homogenizer for 35min under 30 MPa; naturally cooling to room temperature, inspecting, filling into facial mask bags containing facial mask carrier, filling 10g each bag, vacuum drying in microwave vacuum drier for 1.2 hr, and vacuum sealing.
Comparative example 2
A nano plant extract mask comprises the following raw materials in parts by weight: 8 parts of glycerol, 7 parts of 1, 3-butanediol, 0.05 part of dipotassium glycyrrhizinate, 0.18 part of sodium benzoate, 99 parts of water and 6 parts of nano plant extract;
the preparation method of the nano plant extract comprises the following steps:
crushing the dried plant raw materials by a universal crusher, and sieving the crushed plant raw materials by a 100-mesh sieve to obtain plant raw material powder; adding a leaching solution into the plant raw material powder, wherein the mass ratio of the leaching solution to the plant raw material powder is 20:1, uniformly mixing, performing ultrasonic treatment at 80 ℃ for 3 hours, performing ultrasonic power of 800W and ultrasonic frequency of 20kHz, centrifuging, and filtering to obtain a filtrate;
vacuum concentrating the filtrate in 40 deg.C water bath, and drying to obtain plant extract; adding a plant extract into deionized water, wherein the mass ratio of the plant extract to the deionized water is 1:100, ultrasonic dispersion is carried out for 30min, the ultrasonic power is 800W, and the ultrasonic frequency is 20 kHz; homogenizing in a high pressure homogenizer for 35min under 30Mpa, and naturally cooling to room temperature; freezing at-25 deg.C for 12 hr, and freeze drying in a freeze dryer for 72 hr at-58 deg.C;
the leaching liquor is a mixture of ethyl acetate and absolute ethyl alcohol, and the volume ratio of the ethyl acetate to the absolute ethyl alcohol is 2: 1; the plant raw material is carrot;
the preparation method of the nano plant extract mask comprises the following steps: uniformly mixing the raw materials according to a formula, stirring for 30min at 50 ℃, and stirring rotating speed of 300 rpm; homogenizing in a high pressure homogenizer for 35min under 30 MPa; naturally cooling to room temperature, inspecting, filling into facial mask bags containing facial mask carrier, filling 10g each bag, vacuum drying in microwave vacuum drier for 1.2 hr, and vacuum sealing.
Comparative example 3
A nano plant extract mask comprises the following raw materials in parts by weight: 8 parts of glycerol, 7 parts of 1, 3-butanediol, 0.05 part of dipotassium glycyrrhizinate, 0.18 part of sodium benzoate, 99 parts of water and 6 parts of nano plant extract;
the preparation method of the nano plant extract comprises the following steps:
crushing the dried plant raw materials by a universal crusher, and sieving the crushed plant raw materials by a 100-mesh sieve to obtain plant raw material powder; adding a leaching solution into the plant raw material powder, wherein the mass ratio of the leaching solution to the plant raw material powder is 20:1, uniformly mixing, performing ultrasonic treatment at 80 ℃ for 3 hours, performing ultrasonic power of 800W and ultrasonic frequency of 20kHz, centrifuging, and filtering to obtain a filtrate;
vacuum concentrating the filtrate in 40 deg.C water bath, and drying to obtain plant extract; adding a plant extract into deionized water, wherein the mass ratio of the plant extract to the deionized water is 1:100, ultrasonic dispersion is carried out for 30min, the ultrasonic power is 800W, and the ultrasonic frequency is 20 kHz; homogenizing in a high pressure homogenizer for 35min under 30Mpa, and naturally cooling to room temperature; freezing at-25 deg.C for 12 hr, and freeze drying in a freeze dryer for 72 hr at-58 deg.C;
the leaching liquor is a mixture of ethyl acetate and absolute ethyl alcohol, and the volume ratio of the ethyl acetate to the absolute ethyl alcohol is 2: 1; the plant raw material is marigold;
the preparation method of the nano plant extract mask comprises the following steps: uniformly mixing the raw materials according to a formula, stirring for 30min at 50 ℃, and stirring rotating speed of 300 rpm; homogenizing in a high pressure homogenizer for 35min under 30 MPa; naturally cooling to room temperature, inspecting, filling into facial mask bags containing facial mask carriers, filling 10g each bag, vacuum drying in a microwave vacuum drier for 1.2h after filling, and vacuum sealing.
Comparative example 4
A nano plant extract mask comprises the following raw materials in parts by weight: 8 parts of glycerol, 7 parts of 1, 3-butanediol, 0.05 part of dipotassium glycyrrhizinate, 0.18 part of sodium benzoate, 99 parts of water and 6 parts of nano plant extract;
the nano plant extract is a mixture of a nano carrot extract and a nano marigold extract, and the mass ratio of the nano carrot extract to the nano marigold extract is 1: 1;
the preparation method of the nano carrot extract comprises the following steps:
crushing the dried carrots by a universal crusher, and then sieving the crushed carrots by a 100-mesh sieve to obtain carrot powder; adding the leaching liquor into carrot powder, wherein the mass ratio of the leaching liquor to the carrot powder is 20:1, uniformly mixing, performing ultrasonic treatment at 80 ℃ for 3 hours, performing ultrasonic power of 800W and ultrasonic frequency of 20kHz, centrifuging, and filtering to obtain filtrate;
vacuum concentrating the filtrate in 40 deg.C water bath, and drying to obtain radix Dauci Sativae extract; adding a carrot extract into deionized water, wherein the mass ratio of the carrot extract to the deionized water is 1:100, carrying out ultrasonic dispersion for 30min, and carrying out ultrasonic power of 800W and ultrasonic frequency of 20 kHz; homogenizing in a high pressure homogenizer for 35min under 30Mpa, and naturally cooling to room temperature; freezing at-25 deg.C for 12 hr, and freeze drying in a freeze dryer for 72 hr at-58 deg.C;
the leaching liquor is a mixture of ethyl acetate and absolute ethyl alcohol, and the volume ratio of the ethyl acetate to the absolute ethyl alcohol is 2: 1;
the preparation method of the nano marigold extract is the same as that of the nano carrot extract, and the difference is only that the plant raw material is marigold;
the preparation method of the nano plant extract mask comprises the following steps: uniformly mixing the raw materials according to a formula, stirring for 30min at 50 ℃, and stirring rotating speed of 300 rpm; homogenizing in a high pressure homogenizer for 35min under 30 MPa; naturally cooling to room temperature, inspecting, filling into facial mask bags containing facial mask carrier, filling 10g each bag, vacuum drying in microwave vacuum drier for 1.2 hr, and vacuum sealing.
Example 1
A nano plant extract mask comprises the following raw materials in parts by weight: 8 parts of glycerol, 7 parts of 1, 3-butanediol, 0.05 part of dipotassium glycyrrhizinate, 0.18 part of sodium benzoate, 99 parts of water and 6 parts of a nano lipid carrier-plant extract compound;
the preparation method of the nano lipid carrier-plant extract compound comprises the following steps:
adding lecithin and Tween 20 into deionized water, wherein the mass ratio of the lecithin to the deionized water is 1:100, the mass ratio of the Tween 20 to the deionized water is 1.5:100, stirring for 20min at 50 ℃, and stirring at the rotating speed of 300rpm to obtain an aqueous phase solution A;
uniformly mixing glyceryl monostearate and cetyl palmitate, wherein the mass ratio of the glyceryl monostearate to the cetyl palmitate is 4:7, and heating at 76 ℃ for 105 min; sequentially adding vegetable oil and the nano plant extract, uniformly mixing, wherein the mass ratio of the vegetable oil to the cetyl palmitate is 2:1, the mass ratio of the nano plant extract to the cetyl palmitate is 1:1, and continuously heating for 15min at 76 ℃ to obtain an oil phase solution B;
adding the water phase solution A into the oil phase solution B, stirring for 15min at 76 ℃, and stirring at the rotating speed of 300rpm to obtain a mixed phase solution C; homogenizing the mixed phase solution C in a high pressure homogenizer for 35min under the homogenizing pressure of 30Mpa, and naturally cooling to room temperature; freezing at-25 deg.C for 12 hr, and freeze drying in a freeze dryer for 72 hr at-58 deg.C;
the vegetable oil is a mixture of rose hip oil and lemon oil, and the mass ratio of the rose hip oil to the lemon oil is 1: 1;
the nano plant extract is a mixture of a nano carrot extract and a nano marigold extract, and the mass ratio of the nano carrot extract to the nano marigold extract is 1: 1;
the preparation method of the nano carrot extract comprises the following steps:
crushing the dried carrots by a universal crusher, and then sieving the crushed carrots by a 100-mesh sieve to obtain carrot powder; adding the leaching liquor into carrot powder, wherein the mass ratio of the leaching liquor to the carrot powder is 20:1, uniformly mixing, performing ultrasonic treatment at 80 ℃ for 3 hours, performing ultrasonic power of 800W and ultrasonic frequency of 20kHz, centrifuging, and filtering to obtain filtrate;
vacuum concentrating the filtrate in 40 deg.C water bath, and drying to obtain radix Dauci Sativae extract; adding a carrot extract into deionized water, wherein the mass ratio of the carrot extract to the deionized water is 1:100, carrying out ultrasonic dispersion for 30min, and carrying out ultrasonic power of 800W and ultrasonic frequency of 20 kHz; homogenizing in a high pressure homogenizer for 35min under 30Mpa, and naturally cooling to room temperature; freezing at-25 deg.C for 12 hr, and freeze drying in a freeze dryer for 72 hr at-58 deg.C;
the leaching liquor is a mixture of ethyl acetate and absolute ethyl alcohol, and the volume ratio of the ethyl acetate to the absolute ethyl alcohol is 2: 1;
the preparation method of the nano marigold extract is the same as that of the nano carrot extract, and the difference is only that the plant raw material is marigold;
the preparation method of the nano plant extract mask comprises the following steps: uniformly mixing the raw materials according to a formula, stirring for 30min at 50 ℃, and stirring rotating speed of 300 rpm; homogenizing in a high pressure homogenizer for 35min under 30 MPa; naturally cooling to room temperature, inspecting, filling into facial mask bags containing facial mask carrier, filling 10g each bag, vacuum drying in microwave vacuum drier for 1.2 hr, and vacuum sealing.
Comparative example 5
A nano plant extract mask comprises the following raw materials in parts by weight: 8 parts of glycerol, 7 parts of 1, 3-butanediol, 0.05 part of dipotassium glycyrrhizinate, 0.18 part of sodium benzoate, 99 parts of water and 6 parts of a nano lipid carrier-plant extract compound;
the preparation method of the nano lipid carrier-plant extract compound comprises the following steps:
adding lecithin and Tween 20 into deionized water, wherein the mass ratio of the lecithin to the deionized water is 1:100, the mass ratio of the Tween 20 to the deionized water is 1.5:100, stirring for 20min at 50 ℃, and stirring at the rotating speed of 300rpm to obtain an aqueous phase solution A;
uniformly mixing glyceryl monostearate and cetyl palmitate, wherein the mass ratio of the glyceryl monostearate to the cetyl palmitate is 4:7, and heating at 76 ℃ for 105 min; sequentially adding vegetable oil and the nano plant extract, uniformly mixing, wherein the mass ratio of the vegetable oil to the cetyl palmitate is 2:1, the mass ratio of the nano plant extract to the cetyl palmitate is 1:1, and continuously heating for 15min at 76 ℃ to obtain an oil phase solution B;
adding the water phase solution A into the oil phase solution B, stirring for 15min at 76 ℃, and stirring at the rotating speed of 300rpm to obtain a mixed phase solution C; homogenizing the mixed phase solution C in a high pressure homogenizer for 35min under the homogenizing pressure of 30Mpa, and naturally cooling to room temperature; freezing at-25 deg.C for 12 hr, and freeze drying in a freeze dryer for 72 hr at-58 deg.C;
the vegetable oil is a mixture of rose hip oil and lemon oil, and the mass ratio of the rose hip oil to the lemon oil is 1: 1;
the preparation method of the nano plant extract comprises the following steps:
crushing the dried plant raw materials by a universal crusher, and sieving the crushed plant raw materials by a 100-mesh sieve to obtain plant raw material powder; adding a leaching solution into the plant raw material powder, wherein the mass ratio of the leaching solution to the plant raw material powder is 20:1, uniformly mixing, performing ultrasonic treatment at 80 ℃ for 3 hours, performing ultrasonic power of 800W and ultrasonic frequency of 20kHz, centrifuging, and filtering to obtain a filtrate;
vacuum concentrating the filtrate in 40 deg.C water bath, and drying to obtain plant extract; adding a plant extract into deionized water, wherein the mass ratio of the plant extract to the deionized water is 1:100, ultrasonic dispersion is carried out for 30min, the ultrasonic power is 800W, and the ultrasonic frequency is 20 kHz; homogenizing in a high pressure homogenizer for 35min under 30Mpa, and naturally cooling to room temperature; freezing at-25 deg.C for 12 hr, and freeze drying in a freeze dryer for 72 hr at-58 deg.C;
the leaching liquor is a mixture of ethyl acetate and absolute ethyl alcohol, and the volume ratio of the ethyl acetate to the absolute ethyl alcohol is 2: 1; the plant raw material is carrot;
the preparation method of the nano plant extract mask comprises the following steps: uniformly mixing the raw materials according to a formula, stirring for 30min at 50 ℃, and stirring rotating speed of 300 rpm; homogenizing in a high pressure homogenizer for 35min under 30 MPa; naturally cooling to room temperature, inspecting, filling into facial mask bags containing facial mask carrier, filling 10g each bag, vacuum drying in microwave vacuum drier for 1.2 hr, and vacuum sealing.
Comparative example 6
A nano plant extract mask comprises the following raw materials in parts by weight: 8 parts of glycerol, 7 parts of 1, 3-butanediol, 0.05 part of dipotassium glycyrrhizinate, 0.18 part of sodium benzoate, 99 parts of water and 6 parts of a nano lipid carrier-plant extract compound;
the preparation method of the nano lipid carrier-plant extract compound comprises the following steps:
adding lecithin and Tween 20 into deionized water, wherein the mass ratio of the lecithin to the deionized water is 1:100, the mass ratio of the Tween 20 to the deionized water is 1.5:100, stirring for 20min at 50 ℃, and stirring at the rotating speed of 300rpm to obtain an aqueous phase solution A;
uniformly mixing glyceryl monostearate and cetyl palmitate, wherein the mass ratio of the glyceryl monostearate to the cetyl palmitate is 4:7, and heating at 76 ℃ for 105 min; sequentially adding vegetable oil and the nano plant extract, uniformly mixing, wherein the mass ratio of the vegetable oil to the cetyl palmitate is 2:1, the mass ratio of the nano plant extract to the cetyl palmitate is 1:1, and continuously heating for 15min at 76 ℃ to obtain an oil phase solution B;
adding the water phase solution A into the oil phase solution B, stirring for 15min at 76 ℃, and stirring at the rotating speed of 300rpm to obtain a mixed phase solution C; homogenizing the mixed phase solution C in a high pressure homogenizer for 35min under the homogenizing pressure of 30Mpa, and naturally cooling to room temperature; freezing at-25 deg.C for 12 hr, and freeze drying in a freeze dryer for 72 hr at-58 deg.C;
the vegetable oil is a mixture of rose hip oil and lemon oil, and the mass ratio of the rose hip oil to the lemon oil is 1: 1;
the preparation method of the nano plant extract comprises the following steps:
crushing the dried plant raw materials by a universal crusher, and sieving the crushed plant raw materials by a 100-mesh sieve to obtain plant raw material powder; adding a leaching solution into the plant raw material powder, wherein the mass ratio of the leaching solution to the plant raw material powder is 20:1, uniformly mixing, performing ultrasonic treatment at 80 ℃ for 3 hours, performing ultrasonic power of 800W and ultrasonic frequency of 20kHz, centrifuging, and filtering to obtain a filtrate;
vacuum concentrating the filtrate in 40 deg.C water bath, and drying to obtain plant extract; adding a plant extract into deionized water, wherein the mass ratio of the plant extract to the deionized water is 1:100, ultrasonic dispersion is carried out for 30min, the ultrasonic power is 800W, and the ultrasonic frequency is 20 kHz; homogenizing in a high pressure homogenizer for 35min under 30Mpa, and naturally cooling to room temperature; freezing at-25 deg.C for 12 hr, and freeze drying in a freeze dryer for 72 hr at-58 deg.C;
the leaching liquor is a mixture of ethyl acetate and absolute ethyl alcohol, and the volume ratio of the ethyl acetate to the absolute ethyl alcohol is 2: 1; the plant raw material is marigold;
the preparation method of the nano plant extract mask comprises the following steps: uniformly mixing the raw materials according to a formula, stirring for 30min at 50 ℃, and stirring rotating speed of 300 rpm; homogenizing in a high pressure homogenizer for 35min under 30 MPa; naturally cooling to room temperature, inspecting, filling into facial mask bags containing facial mask carrier, filling 10g each bag, vacuum drying in microwave vacuum drier for 1.2 hr, and vacuum sealing.
Example 2
A nano plant extract mask comprises the following raw materials in parts by weight: 8 parts of glycerol, 7 parts of 1, 3-butanediol, 0.05 part of dipotassium glycyrrhizinate, 0.18 part of sodium benzoate, 99 parts of water, 4 parts of a nano lipid carrier-plant extract compound and 2 parts of a functionalized titanium oxide compound;
the preparation method of the nano lipid carrier-plant extract compound comprises the following steps:
adding lecithin and Tween 20 into deionized water, wherein the mass ratio of the lecithin to the deionized water is 1:100, the mass ratio of the Tween 20 to the deionized water is 1.5:100, stirring for 20min at 50 ℃, and stirring at the rotating speed of 300rpm to obtain an aqueous phase solution A;
uniformly mixing glyceryl monostearate and cetyl palmitate, wherein the mass ratio of the glyceryl monostearate to the cetyl palmitate is 4:7, and heating at 76 ℃ for 105 min; sequentially adding vegetable oil and the nano plant extract, uniformly mixing, wherein the mass ratio of the vegetable oil to the cetyl palmitate is 2:1, the mass ratio of the nano plant extract to the cetyl palmitate is 1:1, and continuously heating for 15min at 76 ℃ to obtain an oil phase solution B;
adding the water phase solution A into the oil phase solution B, stirring for 15min at 76 ℃, and stirring at the rotating speed of 300rpm to obtain a mixed phase solution C; homogenizing the mixed phase solution C in a high pressure homogenizer for 35min under the homogenizing pressure of 30Mpa, and naturally cooling to room temperature; freezing at-25 deg.C for 12 hr, and freeze drying in a freeze dryer for 72 hr at-58 deg.C;
the vegetable oil is a mixture of rose hip oil and lemon oil, and the mass ratio of the rose hip oil to the lemon oil is 1: 1;
the nano plant extract is a mixture of a nano carrot extract and a nano marigold extract, and the mass ratio of the nano carrot extract to the nano marigold extract is 1: 1;
the preparation method of the nano carrot extract comprises the following steps:
crushing the dried carrots by a universal crusher, and then sieving the crushed carrots by a 100-mesh sieve to obtain carrot powder; adding the leaching liquor into carrot powder, wherein the mass ratio of the leaching liquor to the carrot powder is 20:1, uniformly mixing, performing ultrasonic treatment at 80 ℃ for 3 hours, performing ultrasonic power of 800W and ultrasonic frequency of 20kHz, centrifuging, and filtering to obtain filtrate;
vacuum concentrating the filtrate in 40 deg.C water bath, and drying to obtain radix Dauci Sativae extract; adding a carrot extract into deionized water, wherein the mass ratio of the carrot extract to the deionized water is 1:100, carrying out ultrasonic dispersion for 30min, and carrying out ultrasonic power of 800W and ultrasonic frequency of 20 kHz; homogenizing in a high pressure homogenizer for 35min under 30Mpa, and naturally cooling to room temperature; freezing at-25 deg.C for 12 hr, and freeze drying in a freeze dryer for 72 hr at-58 deg.C;
the leaching liquor is a mixture of ethyl acetate and absolute ethyl alcohol, and the volume ratio of the ethyl acetate to the absolute ethyl alcohol is 2: 1;
the preparation method of the nano marigold extract is the same as that of the nano carrot extract, and the difference is only that the plant raw material is marigold;
the preparation method of the titanium oxide microspheres comprises the following steps:
dissolving isopropyl titanate in absolute ethyl alcohol, wherein the mass ratio of the isopropyl titanate to the absolute ethyl alcohol is 0.85:1, so as to obtain an isopropyl titanate ethanol solution; dissolving hexadecylamine in absolute ethyl alcohol, wherein the mass ratio of the hexadecylamine to the absolute ethyl alcohol is 1:125, so as to obtain a hexadecylamine ethyl alcohol solution; adding a 0.75 wt% potassium chloride aqueous solution into a hexadecylamine ethanol solution, wherein the mass ratio of the 0.75 wt% potassium chloride aqueous solution to the hexadecylamine ethanol solution is 1:191, and uniformly stirring; adding the isopropyl titanate ethanol solution into the hexadecylamine ethanol solution at the speed of 1mL/min, stirring for 10min at the stirring speed of 300rpm, wherein the mass ratio of the isopropyl titanate ethanol solution to the hexadecylamine ethanol is 1: 16.7; stopping stirring, and standing at 25 ℃ for 18 h; filtering, washing with deionized water for three times, and drying to obtain the final product;
the preparation method of the modified titanium oxide comprises the following steps:
adding the titanium oxide microspheres into deionized water, wherein the mass ratio of the titanium oxide microspheres to the deionized water is 1:20, stirring for 30min at 25 ℃, and the stirring speed is 300 rpm; adding 96.0 wt% chloroacetic acid at the speed of 1mL/min, wherein the mass ratio of the 96.0 wt% chloroacetic acid to the titanium oxide microspheres is 0.2:1, and stirring at the rotating speed of 300rpm for 5 min; then refluxing for 24h at 100 ℃, cooling to room temperature, filtering, washing with deionized water for three times, and drying to obtain the product;
the preparation method of the surface functionalized titanium oxide comprises the following steps:
dissolving 1, 3-dihydroxyacetone dimer in deionized water, wherein the mass ratio of the 1, 3-dihydroxyacetone dimer to the deionized water is 0.5:10, so as to obtain 1, 3-dihydroxyacetone dimer aqueous solution; adding the modified titanium oxide into deionized water, wherein the mass ratio of the modified titanium oxide to the deionized water is 1:20, and stirring for 30min at 25 ℃; adding 98 wt% of sulfuric acid, wherein the mass ratio of the 98 wt% of sulfuric acid to the modified titanium oxide is 0.1: 1; adding 1, 3-dihydroxyacetone dimer aqueous solution, wherein the mass ratio of the 1, 3-dihydroxyacetone dimer aqueous solution to the modified titanium oxide is 10.5:1, stirring for 3h at 100 ℃, and the stirring speed is 300 rpm; cooling to room temperature, filtering, washing with deionized water for three times, and drying to obtain the final product;
the preparation method of the functionalized titanium oxide compound comprises the following steps:
adding the surface functionalized titanium oxide into deionized water, wherein the mass ratio of the surface functionalized titanium oxide to the deionized water is 1:20, and stirring for 30min at 25 ℃; adding arginine, uniformly mixing, stirring at the rotating speed of 300rpm for 6h at the temperature of 80 ℃ and the mass ratio of arginine to surface functionalized titanium oxide of 0.97:1, cooling to room temperature, filtering, washing with deionized water for three times, and drying to obtain the titanium dioxide nano-particles;
the preparation method of the nano plant extract mask comprises the following steps: uniformly mixing the raw materials according to a formula, stirring for 30min at 50 ℃, and stirring rotating speed of 300 rpm; homogenizing in a high pressure homogenizer for 35min under 30 MPa; naturally cooling to room temperature, inspecting, filling into facial mask bags containing facial mask carrier, filling 10g each bag, vacuum drying in microwave vacuum drier for 1.2 hr, and vacuum sealing.
Comparative example 7
A nano plant extract mask comprises the following raw materials in parts by weight: 8 parts of glycerol, 7 parts of 1, 3-butanediol, 0.05 part of dipotassium glycyrrhizinate, 0.18 part of sodium benzoate, 99 parts of water, 4 parts of a nano lipid carrier-plant extract compound and 2 parts of titanium oxide;
the preparation method of the nano lipid carrier-plant extract compound comprises the following steps:
adding lecithin and Tween 20 into deionized water, wherein the mass ratio of the lecithin to the deionized water is 1:100, the mass ratio of the Tween 20 to the deionized water is 1.5:100, stirring for 20min at 50 ℃, and stirring at the rotating speed of 300rpm to obtain an aqueous phase solution A;
uniformly mixing glyceryl monostearate and cetyl palmitate, wherein the mass ratio of the glyceryl monostearate to the cetyl palmitate is 4:7, and heating at 76 ℃ for 105 min; sequentially adding vegetable oil and the nano plant extract, uniformly mixing, wherein the mass ratio of the vegetable oil to the cetyl palmitate is 2:1, the mass ratio of the nano plant extract to the cetyl palmitate is 1:1, and continuously heating for 15min at 76 ℃ to obtain an oil phase solution B;
adding the water phase solution A into the oil phase solution B, stirring for 15min at 76 ℃, and stirring at the rotating speed of 300rpm to obtain a mixed phase solution C; homogenizing the mixed phase solution C in a high pressure homogenizer for 35min under the homogenizing pressure of 30Mpa, and naturally cooling to room temperature; freezing at-25 deg.C for 12 hr, and freeze drying in a freeze dryer for 72 hr at-58 deg.C;
the vegetable oil is a mixture of rose hip oil and lemon oil, and the mass ratio of the rose hip oil to the lemon oil is 1: 1;
the nano plant extract is a mixture of a nano carrot extract and a nano marigold extract, and the mass ratio of the nano carrot extract to the nano marigold extract is 1: 1;
the preparation method of the nano carrot extract comprises the following steps:
crushing the dried carrots by a universal crusher, and then sieving the crushed carrots by a 100-mesh sieve to obtain carrot powder; adding the leaching liquor into carrot powder, wherein the mass ratio of the leaching liquor to the carrot powder is 20:1, uniformly mixing, performing ultrasonic treatment at 80 ℃ for 3 hours, performing ultrasonic power of 800W and ultrasonic frequency of 20kHz, centrifuging, and filtering to obtain filtrate;
vacuum concentrating the filtrate in 40 deg.C water bath, and drying to obtain radix Dauci Sativae extract; adding a carrot extract into deionized water, wherein the mass ratio of the carrot extract to the deionized water is 1:100, carrying out ultrasonic dispersion for 30min, and carrying out ultrasonic power of 800W and ultrasonic frequency of 20 kHz; homogenizing in a high pressure homogenizer for 35min under 30Mpa, and naturally cooling to room temperature; freezing at-25 deg.C for 12 hr, and freeze drying in a freeze dryer for 72 hr at-58 deg.C;
the leaching liquor is a mixture of ethyl acetate and absolute ethyl alcohol, and the volume ratio of the ethyl acetate to the absolute ethyl alcohol is 2: 1;
the preparation method of the nano marigold extract is the same as that of the nano carrot extract, and the difference is only that the plant raw material is marigold;
the preparation method of the titanium oxide microspheres comprises the following steps:
dissolving isopropyl titanate in absolute ethyl alcohol, wherein the mass ratio of the isopropyl titanate to the absolute ethyl alcohol is 0.85:1, so as to obtain an isopropyl titanate ethanol solution; dissolving hexadecylamine in absolute ethyl alcohol, wherein the mass ratio of the hexadecylamine to the absolute ethyl alcohol is 1:125, so as to obtain a hexadecylamine ethyl alcohol solution; adding a 0.75 wt% potassium chloride aqueous solution into a hexadecylamine ethanol solution, wherein the mass ratio of the 0.75 wt% potassium chloride aqueous solution to the hexadecylamine ethanol solution is 1:191, and uniformly stirring; adding the isopropyl titanate ethanol solution into the hexadecylamine ethanol solution at the speed of 1mL/min, stirring for 10min at the stirring speed of 300rpm, wherein the mass ratio of the isopropyl titanate ethanol solution to the hexadecylamine ethanol is 1: 16.7; stopping stirring, and standing at 25 ℃ for 18 h; filtering, washing with deionized water for three times, and drying to obtain the final product;
the preparation method of the nano plant extract mask comprises the following steps: uniformly mixing the raw materials according to a formula, stirring for 30min at 50 ℃, and stirring rotating speed of 300 rpm; homogenizing in a high pressure homogenizer for 35min under 30 MPa; naturally cooling to room temperature, inspecting, filling into facial mask bags containing facial mask carrier, filling 10g each bag, vacuum drying in microwave vacuum drier for 1.2 hr, and vacuum sealing.
Test example 1
Test for patch test on human skin
The test is carried out according to a spot-patch test method of GB 17149-1-1997 general rules of cosmetic skin disease diagnosis and treatment principles, and 93 tested persons meeting the standards are selected. The samples to be tested in the comparative example 1 and the examples 1-2 are put into a spot tester, and 0.02-0.025 mL of sample is added on a filter paper sheet attached to the spot tester by a closed spot test method. Applying the spot tester to the inner side of forearm of a subject by using a non-irritating adhesive tape, wherein one side is a control area and the other side is a test area, lightly pressing with palm to uniformly apply the spot tester to skin, removing the spot tester from the subject after 24h, and observing skin reaction after the indentation disappears; if the result is negative, observing for 1 time after 24h and 48h of the patch test respectively; the blank was deionized water.
TABLE 1 human skin Patch test
Figure BDA0002636035550000161
As can be seen from Table 1, the results of the human skin patch test of the nano extract facial masks prepared in comparative example 1 and examples 1-2 show that the nano extract facial masks have no adverse reaction on human skin and can be safely used.
Test example 2
Anti-inflammatory assay
The anti-inflammatory effect is evaluated by testing the expression inhibition rate of the samples to be tested in comparative examples 1-6 and example 1 on IL-1 beta and TNF-alpha proinflammatory cytokines; subjecting human monocytic leukemia cellsThe strain THP-1 cells were seeded into 24-well cell culture plates each containing 1.0X 106(ii) individual cells; after 72h of activation, adding 1mL of sample to be detected into the cells, and detecting after 18 h; each sample to be tested was paralleled to 3 groups and averaged.
Expression inhibition rate of IL-1 beta proinflammatory cytokine ═ (A-B)/A x 100% formula (1)
Expression inhibition rate of TNF-alpha proinflammatory cytokine (A-B)/A x 100% formula (2)
Wherein A is the expression level without adding the sample to be detected; and B is the expression level of the added test sample.
TABLE 2 inhibition of IL-1 beta, TNF-alpha proinflammatory cytokine expression
Figure BDA0002636035550000171
As can be seen from Table 2, the IL-1 beta and TNF-alpha proinflammatory cytokines of example 1 and comparative examples 5-6 are both smaller than those of comparative examples 1-4; the embodiment 1 and the comparative examples 5 to 6 adopt the nano lipid carrier-plant extract compound, the structure of the nano lipid carrier increases the biocompatibility, and the nano lipid carrier is used as a carrier of a transdermal active ingredient to promote the transdermal absorption of a plant active compound, and simultaneously increases the contact surface with skin cells, so that the plant active ingredient is released more quickly and stably and is absorbed by the skin; therefore, the anti-inflammatory effects of example 1 and comparative examples 5 to 6 were significantly superior to those of comparative examples 1 to 4.
Test example 3
Test for Oxidation resistance test
Carrying out oxidation resistance tests on the samples to be tested in the examples 1-2 and the comparative examples 1-7 by adopting an ABTS method; dissolving ABTS in distilled water to prepare a stock solution 1 of 7.4 mmol/L; dissolving potassium persulfate in distilled water to prepare a stock solution 2 of 2.6 mmol/L; then mixing the stock solution 1 and the stock solution 2 in equal volume, and reacting for 15h at room temperature in a dark place to obtain ABTS working mother liquor; before use, the ABTS solution is diluted to a proper concentration by 80% ethanol (namely, the absorbance value of the diluted ABTS working solution at 734nm is 0.700 +/-0.005). Under the same conditions, the samples to be tested of comparative examples 1 to 7 and examples 1 to 2 were taken for testing, and the samples were paralleled for 3 times and averaged.
Antioxidant activity ═ (a-B)/cx100% formula (3)
Wherein A is the absorbance value of the sample to be detected after reaction, and B is the absorbance value of a blank group without the sample to be detected; c is the absorbance value of the ABTS working solution without sample application.
TABLE 3 Oxidation resistance test Table
Antioxidant activity of%
Comparative example 1 1.6
Comparative example 2 54.3
Comparative example 3 57.8
Comparative example 4 62.4
Example 1 88.5
Comparative example 5 78.2
Comparative example 6 80.1
Example 2 97.7
Comparative example 7 92.9
As can be seen from Table 3, the antioxidant performance of the example 1 and the comparative examples 5-6 (using the nano lipid carrier-plant extract complex) is better than that of the comparative examples 1-4; also, the oxidation resistance of example 2 (adding functionalized titanium oxide composite) is significantly better than that of example 1.
Test example 4
Anti-wrinkle test
The anti-wrinkle effect is evaluated by testing the expression inhibition rate of the samples to be tested in comparative examples 1-7 and examples 1-2 on MMP-1; fibroblasts were seeded into 12-well cell culture plates, each well containing 0.75X 105Carrying out starvation culture on the cells in a serum-free culture medium for 24 hours; after washing the starved cells with PBS buffer, the cells were washed at 312nm and 52mJ/cm2UVB ultraviolet irradiation treatment for 15 s; adding 1mL of sample to be detected into the cells twice in 48 hours; each sample to be tested was paralleled to 3 groups and averaged.
MMP-1 expression inhibition rate ═ (A-B)/A × 100% formula (4)
Wherein A is the expression quantity of MMP-1 after ultraviolet irradiation without adding a sample to be detected; b is the expression quantity of MMP-1 after the sample to be tested is added and is irradiated by ultraviolet.
TABLE 4 MMP-1 expression inhibition
Figure BDA0002636035550000181
Figure BDA0002636035550000191
As can be seen from Table 4, the MMP-1 expression inhibition ratios of example 1 and comparative examples 5-6 (using the nano lipid carrier-plant extract complex) are smaller than those of comparative examples 1-4; the anti-wrinkle effects of example 1 and comparative examples 5-6 are significantly better than those of comparative examples 1-4.
Test example 5
Test of whitening test
Carrying out whitening effect test on the samples to be tested of examples 1-2 and comparative examples 1-7 by adopting a MEXAMETER MX18 skin pigment instrument; selecting 300 healthy tested persons, wherein the tested persons are 22-60 years old, signing an informed consent with the tested persons, measuring the pigment content of the cheeks of the tested persons, and then issuing a sample to be tested; the tested person continuously uses the sample to be tested, the sample is used for 1 time respectively in the morning and at the evening every day, and the sample is applied after face cleaning; other whitening cosmetics were discontinued during the experiment; after continuously using 7d, 14d, 21d and 28d, determining each efficacy index by the same method; testing the ambient temperature (22 +/-1) DEG C and the humidity (50 +/-5)%, and carrying out real-time dynamic monitoring; continuously testing for 3 times, and taking an average value; the blank control is that the test sample and other whitening cosmetics are not used during the experiment.
Melanin reduction rate ═ a-B)/ax100% formula (5)
Wherein A is the melanin content of the test sample which is not used at the beginning of the test; and B is the melanin content after the test sample is used.
TABLE 5 Melanin reduction
Figure BDA0002636035550000192
Figure BDA0002636035550000201
Figure BDA0002636035550000211
Compared with the blank group, the test results P of the samples to be tested of the comparative examples 2-7 and the examples 1-2 are less than 0.05.
As can be seen from table 5, the melanin reduction rates of example 2 and comparative example 7 were superior to those of example 1; also, the melanin reduction rate of example 2 (increased functionalized titanium oxide complex) was significantly better than that of comparative example 7 (increased titanium oxide). Example 2 adopts a functionalized titanium oxide compound, the specific surface area and the ultraviolet protection function of the compound are enhanced, and the thermal stability and the light stability of the compound are higher; further, the whitening effect of example 2 is better than that of comparative example 7.
Test example 6
Test of moisture retention test
A CUK skin tester is adopted to test the moisturizing effect of the samples to be tested in the embodiment 1 and the comparative examples 1-6; selecting 150 healthy tested persons, wherein the tested persons are 20-40 years old, signing an informed consent with the tested persons, measuring the skin humidity of the tested persons, and then issuing a sample to be tested; the tested person continuously uses the sample to be tested, the sample is used for 1 time respectively in the morning and at the evening every day, and the sample is applied after face cleaning; other moisturizing cosmetics were discontinued during the experiment; after continuously using 7d, 14d, 21d and 28d, determining each efficacy index by the same method; testing the ambient temperature (22 +/-1) DEG C and the humidity (50 +/-5)%, and carrying out real-time dynamic monitoring; continuously testing for 3 times, and taking an average value; blank control is no test sample and other moisturizing cosmetics used during the experiment.
Skin moisture increase rate ═ (a-B)/a × 100% formula (6)
Wherein A is the skin humidity of the sample to be tested which is not used at the beginning of the test; and B is the skin humidity after the test sample is used.
TABLE 6 rate of skin moisture increase
Figure BDA0002636035550000212
Figure BDA0002636035550000221
Compared with the blank group, the test results P of the samples to be tested in comparative examples 2-6 and example 1 are less than 0.05.
As can be seen from table 6, the skin moisture increase rate of example 1 (using the nano lipid carrier-plant extract complex) was superior to that of comparative example 4.
The foregoing detailed description of the preferred embodiments of the invention has been presented. It should be understood that numerous modifications and variations could be devised by those skilled in the art in light of the present teachings without departing from the inventive concepts. Therefore, the technical solutions available to those skilled in the art through logic analysis, reasoning and limited experiments based on the prior art according to the concept of the present invention should be within the scope of protection defined by the claims.

Claims (10)

1. The nano plant extract mask is characterized by comprising the following raw materials in parts by weight: 1-10 parts of glycerol, 1-10 parts of 1, 3-butanediol, 0.01-0.2 part of dipotassium glycyrrhizinate, 0.01-0.5 part of sodium benzoate, 95-155 parts of water and 1-10 parts of nano plant extract.
2. The nano plant extract mask is characterized by comprising the following raw materials in parts by weight: 1-10 parts of glycerol, 1-10 parts of 1, 3-butanediol, 0.01-0.2 part of dipotassium glycyrrhizinate, 0.01-0.5 part of sodium benzoate, 95-155 parts of water and 1-10 parts of nano lipid carrier-plant extract compound.
3. The nano plant extract mask is characterized by comprising the following raw materials in parts by weight: 1-10 parts of glycerol, 1-10 parts of 1, 3-butanediol, 0.01-0.2 part of dipotassium glycyrrhizinate, 0.01-0.5 part of sodium benzoate, 95-155 parts of water, 1-10 parts of a nano lipid carrier-plant extract compound and 1-10 parts of a functionalized titanium oxide compound.
4. The nano plant extraction mask of claim 2 or 3, wherein: the preparation method of the nano lipid carrier-plant extract compound comprises the following steps:
adding lecithin and Tween 20 into deionized water, wherein the mass ratio of the lecithin to the deionized water is (0.5-10): 100-200), the mass ratio of the Tween 20 to the deionized water is (0.5-10): 100-200), stirring for 5-60min at 10-60 ℃, and stirring at the rotating speed of 50-500rpm to obtain an aqueous phase solution A;
uniformly mixing glyceryl monostearate and cetyl palmitate, wherein the mass ratio of the glyceryl monostearate to the cetyl palmitate is (1-10) to (1-20), and heating at 30-100 ℃ for 20-200 min; sequentially adding vegetable oil and nano plant extract, uniformly mixing, wherein the mass ratio of the vegetable oil to the cetyl palmitate is (1-10) to (0.5-5), the mass ratio of the nano plant extract to the cetyl palmitate is (0.1-5) to (0.1-5), and continuously heating at 30-100 ℃ for 10-60min to obtain an oil phase solution B;
adding the water phase solution A into the oil phase solution B, continuously heating at 30-100 deg.C for 10-60min, and stirring at 50-500rpm to obtain mixed phase solution C; homogenizing the mixed phase solution C in a high pressure homogenizer for 5-60min under the homogenizing pressure of 5-60Mpa, and naturally cooling to room temperature; freezing at- (5-30) deg.C for 1-24 hr, lyophilizing in a lyophilizer for 12-96 hr, and setting the temperature at- (5-70) deg.C.
5. The nano-implant extraction mask of claim 4, wherein: the vegetable oil is at least one of rosehip oil, lemon oil and grape seed oil.
6. The nano plant extract mask as claimed in claim 5, wherein: the vegetable oil is a mixture of rose hip oil and lemon oil, and the mass ratio of the rose hip oil to the lemon oil is (0.1-5) to (0.1-5).
7. The nano plant extraction mask of claim 1 or 4, wherein: the preparation method of the nano plant extract comprises the following steps:
crushing the dried plant raw materials by a universal crusher, and sieving by a sieve of 20-200 meshes to obtain plant raw material powder; adding a leaching solution into the plant raw material powder, wherein the mass ratio of the leaching solution to the plant raw material powder is (1-100):1, uniformly mixing, carrying out ultrasonic treatment at 20-100 ℃ for 0.5-5h, wherein the ultrasonic power is 500 plus one hundred thousand (W) and the ultrasonic frequency is 20-100kHz, centrifuging, and filtering to obtain a filtrate;
vacuum concentrating the filtrate in 20-60 deg.C water bath, and drying to obtain plant extract; adding a plant extract into deionized water, wherein the mass ratio of the plant extract to the deionized water is 1 (10-200), ultrasonic dispersion is carried out for 5-60min, the ultrasonic power is 500-1000W, and the ultrasonic frequency is 20-100 kHz; homogenizing in a high pressure homogenizer for 5-60min under 5-60Mpa, and naturally cooling to room temperature; freezing at- (5-30) deg.C for 1-24 hr, lyophilizing in a lyophilizer for 12-96 hr, and setting the temperature at- (5-70) deg.C.
8. The nano-implant extraction mask of claim 7, wherein: the leaching liquor is a mixture of ethyl acetate and absolute ethyl alcohol, and the volume ratio of the ethyl acetate to the absolute ethyl alcohol (0.5-10) is 1.
9. The nano-implant extraction mask of claim 7, wherein: the plant material is at least one of carrot, cucumber, agaric, wolfberry fruit and marigold.
10. The method for preparing a nano plant extraction mask as claimed in any one of claims 1 to 9, comprising the steps of:
mixing the raw materials uniformly according to the formula, stirring for 5-60min at 20-60 ℃, and stirring speed of 50-500 rpm; homogenizing for 5-60min under 5-60 Mpa; naturally cooling to room temperature, inspecting, filling into facial mask bags containing facial mask carrier, filling 1-20g each bag, vacuum drying for 0.5-5 hr after filling, and vacuum sealing.
CN202010825441.0A 2020-08-17 2020-08-17 Nano plant extract mask and preparation method thereof Withdrawn CN111870571A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202010825441.0A CN111870571A (en) 2020-08-17 2020-08-17 Nano plant extract mask and preparation method thereof

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202010825441.0A CN111870571A (en) 2020-08-17 2020-08-17 Nano plant extract mask and preparation method thereof

Publications (1)

Publication Number Publication Date
CN111870571A true CN111870571A (en) 2020-11-03

Family

ID=73202752

Family Applications (1)

Application Number Title Priority Date Filing Date
CN202010825441.0A Withdrawn CN111870571A (en) 2020-08-17 2020-08-17 Nano plant extract mask and preparation method thereof

Country Status (1)

Country Link
CN (1) CN111870571A (en)

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114796055A (en) * 2022-05-19 2022-07-29 广东轻工职业技术学院 Whitening dressing rich in liposome nanoparticles and preparation method thereof
CN115227628A (en) * 2022-09-03 2022-10-25 深圳青春一九美业管理有限公司 Biological peptide skin care solution for whitening, resisting wrinkles and tendering skin and preparation method thereof
CN115501151A (en) * 2022-10-10 2022-12-23 广东工业大学 Tearable potato soft mask powder with whitening effect and preparation method thereof

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106924073A (en) * 2017-05-09 2017-07-07 南通千竹电子科技有限公司 A kind of replenishing water and preserving moisture facial mask and preparation method thereof
CN109172500A (en) * 2018-09-27 2019-01-11 南通蛇类治疗研究所 Nanometer plants extraction facial mask
CN110693800A (en) * 2019-11-27 2020-01-17 杭州梵歌生物科技有限公司 Nano plant extract mask and preparation method thereof
CN110882198A (en) * 2019-10-17 2020-03-17 广州熠辉生物科技有限公司 Antibacterial moisturizing and whitening mask and preparation method thereof

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106924073A (en) * 2017-05-09 2017-07-07 南通千竹电子科技有限公司 A kind of replenishing water and preserving moisture facial mask and preparation method thereof
CN109172500A (en) * 2018-09-27 2019-01-11 南通蛇类治疗研究所 Nanometer plants extraction facial mask
CN110882198A (en) * 2019-10-17 2020-03-17 广州熠辉生物科技有限公司 Antibacterial moisturizing and whitening mask and preparation method thereof
CN110693800A (en) * 2019-11-27 2020-01-17 杭州梵歌生物科技有限公司 Nano plant extract mask and preparation method thereof

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114796055A (en) * 2022-05-19 2022-07-29 广东轻工职业技术学院 Whitening dressing rich in liposome nanoparticles and preparation method thereof
CN114796055B (en) * 2022-05-19 2023-08-15 广东艾粒生物科技有限责任公司 Whitening dressing rich in liposome nanoparticles and preparation method thereof
CN115227628A (en) * 2022-09-03 2022-10-25 深圳青春一九美业管理有限公司 Biological peptide skin care solution for whitening, resisting wrinkles and tendering skin and preparation method thereof
CN115501151A (en) * 2022-10-10 2022-12-23 广东工业大学 Tearable potato soft mask powder with whitening effect and preparation method thereof
CN115501151B (en) * 2022-10-10 2024-01-16 广东工业大学 Tear-off potato soft film powder with whitening effect and preparation method thereof

Similar Documents

Publication Publication Date Title
CN111870571A (en) Nano plant extract mask and preparation method thereof
WO2018113448A1 (en) Jasmine essence nutritional skincare aloe vera gel
CN111920730A (en) Repairing moisturizing cream and preparation method thereof
CN115040461A (en) Moisturizing and hydrating fresh freeze-dried mask
WO2018113446A1 (en) Rose essence nutritional skincare aloe vera gel
CN110559222B (en) Moisturizing antioxidant gel and preparation method thereof
CN111759774A (en) Whitening anti-wrinkle essence
JP5770428B2 (en) Singlet oxygen scavenger, skin external preparation and cosmetic using the singlet oxygen scavenger
CN109223607B (en) Anti-wrinkle moisturizing skin-brightening composition and cosmetic
CN112089666A (en) Antioxidant composition and preparation method and application thereof
CN111297733A (en) Paeonol-containing high-moisture-retention sun-screening agent and preparation method thereof
WO2018113445A1 (en) Rosa chinensis essence nutritional skincare aloe vera gel
CN115177975A (en) A method for extracting polysaccharides, polyphenols and triterpenes from medicinal fomes fomentarius by supramolecular process
CN108852999A (en) A kind of formula and technique of Xinhui citrus reticulata flower extract liquor production facial mask
CN114931523A (en) Moistening, whitening and moisturizing essence and preparation method thereof
JP2011168543A (en) Singlet oxygen scavenger, and skin care external preparation and cosmetic each using the singlet oxygen scavenger
CN112107494A (en) Facial mask essence
CN112494408A (en) Whitening and inflammation diminishing mask liquid and preparation method thereof
CN110946776A (en) A skin caring cream containing cicada extract and its preparation method
CN115624510B (en) Whitening essence and preparation method thereof
CN118021647B (en) Cosmetic skin care mask containing hirudin and preparation method thereof
KR102494394B1 (en) Composition comprising fermented extract from pine for preventing skin wrinkle, improving skin barrier function, preventing hair loss, promoting hair growth and improving hair health and method for manufacturing the same
CN113318032B (en) Anti-aging moisturizing cosmetic and preparation method thereof
TWI787623B (en) A cosmetic composition for preventing and/or improving skin aging and its application
CN110742833B (en) Acne-removing, whitening and anti-aging essential oil composition as well as preparation method and application thereof

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
WW01 Invention patent application withdrawn after publication

Application publication date: 20201103

WW01 Invention patent application withdrawn after publication