CN111419760A - Fresh black tiger leaf extracting solution and preparation method and application thereof - Google Patents
Fresh black tiger leaf extracting solution and preparation method and application thereof Download PDFInfo
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- CN111419760A CN111419760A CN202010382906.XA CN202010382906A CN111419760A CN 111419760 A CN111419760 A CN 111419760A CN 202010382906 A CN202010382906 A CN 202010382906A CN 111419760 A CN111419760 A CN 111419760A
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Classifications
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/96—Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution
- A61K8/97—Cosmetics 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
- A61K8/9783—Angiosperms [Magnoliophyta]
- A61K8/9789—Magnoliopsida [dicotyledons]
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/96—Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution
- A61K8/97—Cosmetics 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
- A61K8/9783—Angiosperms [Magnoliophyta]
- A61K8/9794—Liliopsida [monocotyledons]
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
- A61Q19/00—Preparations for care of the skin
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
- A61Q19/00—Preparations for care of the skin
- A61Q19/02—Preparations for care of the skin for chemically bleaching or whitening the skin
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
- A61Q19/00—Preparations for care of the skin
- A61Q19/08—Anti-ageing preparations
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
- A61Q19/00—Preparations for care of the skin
- A61Q19/10—Washing or bathing preparations
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2800/00—Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
- A61K2800/80—Process related aspects concerning the preparation of the cosmetic composition or the storage or application thereof
- A61K2800/805—Corresponding aspects not provided for by any of codes A61K2800/81 - A61K2800/95
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2800/00—Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
- A61K2800/80—Process related aspects concerning the preparation of the cosmetic composition or the storage or application thereof
- A61K2800/85—Products or compounds obtained by fermentation, e.g. yoghurt, beer, wine
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)
- Dermatology (AREA)
- Biotechnology (AREA)
- Engineering & Computer Science (AREA)
- Botany (AREA)
- Microbiology (AREA)
- Mycology (AREA)
- Birds (AREA)
- Epidemiology (AREA)
- Gerontology & Geriatric Medicine (AREA)
- Cosmetics (AREA)
Abstract
The invention discloses an extracting solution which is extracted from fresh black tiger leaves and has multiple effects of skin tendering, wrinkle resistance, whitening and the like. The black tiger is called 'third generation health preserving miracle fruit' with a very low price; fresh leaves are thick and juicy and are rich in various skin care components, and the juice obtained after mashing is a good bath product which is handed over between mouths of young people in the southwest of China, Dong and other minority women, but the juice has high viscosity and is difficult to process and apply by adopting processes such as filtration and the like. The invention discloses a multi-step gel breaking process for sterilization, pulping, enzymolysis, probiotic fermentation, extraction, precipitation and the like at room temperature, which can decompose macromolecules such as vegetable protein, cellulose and the like contained in the gel breaking process into micromolecular peptides and ferment with beauty treatment efficacy, and finally obtain a clear fresh black tiger leaf extracting solution. The fragrant facial cleanser with the functions of cleaning face, moistening skin, resisting wrinkles and removing freckles can be prepared by taking the extract as a main component and adding water, cocamidopropyl betaine, sodium cocoyl glycinate, glycerol and the like.
Description
Technical Field
The invention relates to the technical field of comprehensive utilization of black tiger resources, in particular to a black tiger fresh leaf extracting solution and a preparation method and application thereof.
Background
The black tiger is a evergreen vine plant of the genus Kadsura of the family Schisandraceae, the leaf of which is flat boat-shaped, large and fat, has fragrant and pleasant smell, is rich in various colloids, plant essential oil, vegetable protein, natural emulsifier and surfactant, and is taken down and slightly kneaded and squeezed to obtain fresh juice, namely a bathing product which is popular among minority women, such as seedlings and Dong people in southwest of China, has the effects of cleaning face, tendering skin, removing freckles, removing wrinkles and powerful whitening and antioxidation effects, and can make the skin transparent and white in common use. However, because of the limitations of various conditions, it has been reported that it is applied to the preparation of cosmetic or bath material in large scale.
The black tiger fruit is also called as Bufna in Miao nationality, which means the beauty-maintaining and longevity fruit. Researches show that the health-care food is rich in various amino acids, vitamins, anthocyanin, polyphenol, pectin, lignan and the like, is beneficial to human bodies, and is called 'third-generation health-care miracle fruit' with great development value. At present, scholars use the extract of the black tiger fruit as a raw material of cosmetics, but the market price of the black tiger fruit is higher at present, and the supply is difficult to guarantee. In fact, for the skin, most of beneficial active ingredients contained in the fruits also exist in the fresh leaves, the price of the fresh leaves is often less than one twentieth or even one hundredth of that of the black tiger fruits, and the black tiger fruits can be picked all the year round without being limited by seasons for picking the fresh fruits, so that the raw materials using the fresh black tiger leaves have greater economic benefit and practicability for the cosmetic industry than the fresh fruits.
The rhizome of kadsura coccinea is commonly called as sargentgloryvine stem, is an important Chinese medicinal material, has the effects of setting fracture, dissipating blood stasis, reducing swelling and detoxifying in Luchuan herbal medicine, and is commonly used for treating traumatic fracture, rheumatic ostealgia, sore and furuncle, wound infection and the like. Obviously, the extract of the plant extract also has certain effects of promoting blood circulation and beautifying if being used in cosmetics. However, the most distinctive and most essential part of the black tiger, including volatile plant essential oil and other natural small molecule active ingredients with the functions of cleaning face, moistening skin and beautifying, is not basically existed in the dried root and stem of the black tiger. On the contrary, the effective components such as lignans, triterpenes, amino acids and the like with the effects of promoting blood circulation and beautifying contained in the rhizome of the tiger also exist in the fresh leaf of the tiger. In other words, the fresh black tiger leaves are obviously more advantageous than the rhizomes if used as raw materials of cosmetics and bath products because they contain more active ingredients with remarkable efficacies including plant essential oils. In addition, compared with the rhizome of the black tiger, the fresh leaf of the black tiger has another great advantage that the rhizome of the black tiger is dug, so that the destructive exploitation of the precious natural resources of the black tiger is often caused, and the price of the black tiger is further increased continuously. In contrast, the normal growth of the plants cannot be damaged as long as the fresh black tiger leaves are picked with a little attention, and the fresh black tiger leaves can be picked all the year round according to the production requirements, so that the method is economical and environment-friendly, and a green and sustainable development mode of the natural black tiger resources is formed.
However, it has proven to be difficult to extract a pleasant, sparkling and clear extract from the fresh leaves of Kadsura coccinea, which is a fundamental requirement for higher-grade bath or cosmetic materials. The method is characterized in that the fresh black tiger leaves contain a large amount of active ingredients such as colloid, plant essential oil, plant protein and polysaccharide, so that a colloidal solution wrapping a large amount of fine plant fiber suspended matters is formed once the fresh black tiger leaves are crushed, and colloidal particles in the colloidal solution have extremely high viscosity and can be stuck to various filters, so that the filtration cannot be carried out. To put it back, even if filtration is possible, since these viscous colloidal particles encapsulate a lot of valuable active ingredients, if all are discarded as filter residue, a large amount of active ingredients are lost. The extraction of the fresh black tiger leaves is easy to say, and the real operation is very difficult. Therefore, it is very important to provide a fresh black tiger leaf extract which has low viscosity and high clarity and has no damage to the effective components during extraction and apply the extract to high-grade cosmetics.
Disclosure of Invention
The first purpose of the invention is to fully utilize a high-quality and low-price natural resource, namely the fresh black tiger leaves, and design a set of technical scheme, so that the stability of a colloidal solution naturally formed after the fresh black tiger leaves are crushed can be effectively broken, and an extracting solution which is fragrant, pleasant, crystal clear, tender, anti-wrinkle, antioxidant, freckle-removing, whitening and the like is further extracted, so that waste is changed into valuable, and the sustainable utilization of natural resources is realized.
The second purpose of the invention is to provide a faint scent type facial cleanser prepared by the extracting solution; and other bathing or cosmetic methods with higher grade.
The technical scheme provided by the invention is based on the basic principle that the effective components in the fresh black tiger leaves are extracted to the maximum extent, and the effective components are ensured not to be damaged in the extraction process as much as possible. Therefore, strict temperature control is necessary and the entire extraction process must be kept below 40 degrees celsius.
In order to achieve the first object, the invention adopts the technical scheme that the method comprises the following operation steps:
s1, collecting: selecting fresh black tiger leaves as a raw material; the fresh black tiger leaves are large and thick, and only dozens of pieces are needed to be one kilogram. It is better to collect enough processing amount in the same day in the early morning according to the plan, but not to collect more. And the sustainable growth of the black tiger plants is protected, and each vine man needs to keep a certain amount of fresh leaves when needing to be kept;
s2, disinfection and sterilization: if the fresh leaves are stained with silt, the silt can be simply washed away by clear water, the fresh leaves are naturally dried in a shady and ventilated place, then ozone is introduced into a sealing bag for about 5-10 min, and simple sterilization and disinfection treatment is carried out to prepare for the subsequent fermentation and enzymolysis procedures;
s3, crushing and pulping: chopping the sterilized fresh black tiger leaves, putting into a wall breaking machine, adding water, and crushing into pulp to obtain the original pulp of the fresh black tiger leaves; the crushing of the fresh leaves can not be realized by the method of drying and crushing the Chinese herbal medicines which is commonly used, the low temperature can be kept only by wet pulping, and the effective components are kept and are not damaged. The specific operation is that firstly, the sterilized fresh leaves are cut into a plurality of sections, and then the fresh leaves are put into a fruit and vegetable wall breaking machine; adding purified water with the weight of one to two times of the leaves, starting a wall breaking machine to break the fresh leaves into pulp; the opening time of a high-speed gear of the wall breaking machine is controlled, and the opening time is not more than 20 seconds each time, so that the loss of effective components caused by local high temperature is avoided;
s4, primary gel breaking: adding a complex enzyme for primary gel breaking, stirring, carrying out enzymolysis reaction at 35-38 ℃, reacting for 3-7 h, standing, and separating supernatant and lower-layer colloidal solution, wherein the supernatant is stored at 4-8 ℃ to obtain primary extract A.
The fresh black tiger leaves contain a large amount of colloid components, pectin, lignan and the like, and a colloid solution with certain viscosity is formed after water is added and the fresh black tiger leaves are crushed; in order to extract the effective components and separate and discard a large amount of useless plant fibers, the stability of the colloidal solution must be firstly broken. Therefore, the invention designs a special process for three-time gel breaking; the first gel breaking is carried out by means of biological enzymolysis, namely adding specially designed complex enzyme into colloidal solution for enzymolysis reaction. The composition of the complex enzyme added for the primary gel breaking is as follows: cellulase, pectinase and papain, wherein the mass ratio of the cellulase to the pectinase to the papain is 2: 1: 1; the adding amount is 0.1-0.3% of the total amount of the colloidal solution, the colloidal solution is fully stirred after being added, and the temperature of the enzymolysis reaction is controlled between 35 ℃ and 38 ℃. The time of the enzymolysis reaction is 3-7 hours. The main effect of enzymolysis is to decompose a large amount of vegetable protein and cellulose contained in the colloid into small molecular peptides and other small molecular components with high activity and good cosmetic effect. Meanwhile, the structure of colloidal particles is also destroyed, so that the original extremely turbid solution obviously obtains a certain degree of clarification, particularly the upper half part of the solution. At this time, a siphon tube or a container for holding the solution is inclined, one third to one half of the clarified solution at the upper part is transferred into another container, and then the clarified solution is sealed and stored at low temperature and is marked as primary extracting solution A;
s5, secondary gel breaking: and taking the lower-layer colloidal solution, adding probiotics, stirring to obtain a fermentation liquid, fermenting for 3-7 days at 20 ℃, and filtering to obtain a primary extracting solution B and a solid filter cake.
Although the solution before secondary gel breaking is still turbid, through the action of complex enzyme, a plurality of active ingredients which are originally adhered with plant fibers are effectively separated, some cellulose and starch are decomposed into sugar, and some protein is also decomposed into small peptide and amino acid by protease, which exactly provides reliable energy, carbon source and nitrogen source for the growth of fermentation microorganisms. The secondary gel breaking of the invention adopts a method of adding probiotics for fermentation, so that a large amount of complex macromolecular compounds in the solution are decomposed into beneficial components with small molecular weight and capable of directly penetrating into the skin under the action of the probiotics and various fresh proteases secreted by the probiotics, and the structure of colloid particles is changed at the same time, and the stability of colloid is damaged. Certainly, the solution also contains a certain amount of enzymes produced by probiotics, namely various enzymes capable of promoting the growth of skin cells, removing blood stasis, expelling toxin and other physiological functions, so the final extract can be named as 'black tiger enzyme';
s6, alcohol extraction: according to the invention, the solid filter cake separated in the secondary gel breaking process still contains some components which have poor hydrophilicity and are still beneficial to skin, such as anthocyanin and the like, in order to fully recover the components, the solid filter cake in the step S5 is crushed, 95% ethanol solution is added for extraction, the mixture is stirred for 1-2 hours at the temperature of 30-35 ℃, and the primary extracting solution C is obtained by filtration;
s7, third gel breaking: the primary extract A and the primary extract B obtained by the method still contain a plurality of tiny colloidal particles which are composed of a plurality of tiny plant fibers, plant protein fragments, amino acids and the like, and the surfaces of the tiny plant fibers, the tiny plant protein fragments, the tiny amino acids and the tiny vegetable protein fragments have a plurality of hydrophilic polar groups such as amino groups, carboxyl groups, hydroxyl groups and the like; thus, hydration is easy to occur, and a thicker hydration layer is formed; the particles are isolated from each other and cannot aggregate to form a precipitate. To break the stability of such colloidal solutions, the hydration layer around the colloidal particles is first broken. Applicants have found that adjusting the pH of the solution can alter the thickness of the hydration layer; the organic extractant ethanol has strong hydrophilic ability and can be used as a dehydrating agent to destroy a hydration layer on the periphery of the colloid particles. Thus, the purpose of breaking the stability of the colloid can be achieved by the two pipes. Therefore, the applicant mixes the primary extracting solution A and the primary extracting solution B, adjusts the pH value to 6.5-7.5, adds the primary extracting solution C, stirs, stands, and takes supernatant after precipitation;
s8, ultramicro membrane filtration: and (5) carrying out ultramicro membrane filtration on the supernatant obtained in the step S7 to obtain a fresh black tiger leaf extracting solution. According to the invention, the supernatant separated after 3 times of gel breaking is not clear enough, but completely different from the supernatant before treatment, and can not block various filter nets or membranes. At this time, the domestic ultra-micro filter membrane sterilization filter can be conveniently used for filtering the obtained supernatant; thereby obtaining a completely sterile fresh black tiger leaf extract with crystal clear appearance and pleasant fragrance;
further, in the step S3, the weight ratio of the sterilized fresh black tiger leaves to water is 1: 1 to 2.
Further, in the step S4, the mass of the compound enzyme is 0.1-0.3% of the original black tiger fresh leaf pulp, and the compound enzyme is prepared from cellulose, pectinase and papain in a ratio of 2: 0.5-2: 0.5-2 mass ratio.
Preferably, in the step S4, the mass of the complex enzyme is 0.2% of the original black tiger fresh leaf pulp, and the complex enzyme is prepared from cellulose, pectinase and papain in a ratio of 2: 1: 1, in terms of mass ratio.
Further, in the step S5, the probiotics is selected from special yeast for Angel wine fruit wine, and the mass of the probiotics is 0.05-0.2% of the mass of the lower layer colloidal solution.
Preferably, in the step S5, the probiotics is selected from special yeast for Angel wine, and the mass of the probiotics is 0.12% of the mass of the lower layer colloid solution.
Further, in the step S5, white granulated sugar is added to the fermentation broth the next day after the fermentation starts, and the addition amount of the white granulated sugar is 0.2 to 0.5% of the total weight of the fermentation broth.
Preferably, in the step S5, white granulated sugar is added into the fermentation broth the next day after the fermentation starts, and the addition amount of the white granulated sugar is 0.3% of the total weight of the fermentation broth.
Further, in the step S6, the weight ratio of the solid filter cake to the 95% ethanol solution is 1: 1 to 2.
Preferably, further, in the step S6, the weight ratio of the solid filter cake to the 95% ethanol solution is 1: 2.
the fresh black tiger leaf extract can be used for preparing cosmetics with whitening and freckle removing functions, and the cosmetics comprise paste, emulsion, film, spray, gel or soap.
The invention also provides facial cleanser containing the fresh black tiger leaf extract, which comprises the following components in parts by weight: 15-30 parts of fresh black tiger leaf extracting solution, 20-25 parts of deionized water, 3-5 parts of cocamidopropyl betaine, 2-4 parts of sodium cocoyl glycinate, 8-10 parts of glycerol, 25-30 parts of sodium methyl cocoyl taurate, 1-1.5 parts of PEG-250 distearate, 1.5-2 parts of sodium chloride, 0.03-0.05 part of disodium EDTA, 0.05-0.1 part of soothing and moisturizing extracting solution, 0.3-0.5 part of caprylyl hydroximic acid, 0.2-0.3 part of glyceryl caprylate, 0.1-0.2 part of propylene glycol and 0.05-0.1 part of essence.
Further, the soothing and moisturizing extracting solution is an aloe extracting solution or a witch hazel extracting solution.
Preferably, the facial cleanser with the fresh black tiger leaf extracting solution comprises the following components in parts by weight: 20 parts of a fresh black tiger leaf extracting solution, 30 parts of deionized water, 4 parts of cocamidopropyl betaine, 4 parts of sodium cocoyl glycinate, 8 parts of glycerol, 30 parts of sodium methyl cocoyl taurate, 1.5 parts of PEG-250 distearate, 2 parts of sodium chloride, 0.05 part of EDTA disodium, 0.1 part of a witch hazel extracting solution, 0.4 part of caprylyl hydroximic acid, 0.25 part of glyceryl caprylate, 0.15 part of propylene glycol and 0.05 part of a florist essence, wherein the florist essence is derived from Youran biotechnology, Guangzhou.
The invention also provides a preparation method of the facial cleanser containing the fresh black tiger leaf extract, which comprises the following steps:
a1, mixing deionized water, cocamidopropyl betaine, sodium cocoyl glycinate, glycerol, sodium methyl cocoyl taurate and EDTA disodium according to the formula ratio, and stirring at 80-85 ℃ until the mixture is transparent;
a2, cooling to 60 ℃, adding PEG-250 distearate with the formula amount, and stirring uniformly;
a3, cooling to 50 ℃, adding a sodium chloride solution, and stirring; wherein the sodium chloride solution is a pre-dissolved saturated aqueous solution of sodium chloride;
a4, cooling to 45 ℃, adding the formula amount of the fresh black tiger leaf extract, the soothing and moisturizing extract, the essence, and the pre-dispersed caprylyl hydroximic acid, glyceryl caprylate and propylene glycol; stirring, cooling and standing to obtain the final product.
The fresh black tiger leaf extracting solution and the preparation method thereof have the following beneficial effects:
(1) the invention adopts the fresh black tiger leaves as the raw material of the fresh black tiger leaf extracting solution, reserves the fresh fruits and the rattan, and only collects the fresh leaves intermittently at intervals, thereby realizing the road of utilizing the black tiger resources in sustainable development.
(2) The invention adopts advanced biological enzymolysis and fermentation technology, successfully decomposes and converts a large amount of components such as vegetable protein, colloid, cellulose and the like contained in the fresh black tiger leaves into a plurality of small molecular peptides and a plurality of enzymes which are beneficial to the skin and are easy to absorb, and simultaneously destroys the structure of colloid particles, so that the original extremely turbid solution is obviously clarified to a certain degree, and the medicinal efficacy of the black tiger is greatly expanded; in addition, as the process adopted by the preparation method of the fresh black tiger leaf extracting solution is operated at room temperature, a plurality of active ingredients such as black tiger essential oil, anthocyanin, vitamin and the like which cannot be reserved even along with traditional black tiger traditional Chinese medicinal materials are reserved, and the unique faint scent of the black tiger is reserved.
(3) In the three gel breaking process steps, the pH value of the mixed solution of the primary extracting solution A and the primary extracting solution B is adjusted, and the primary extracting solution C containing ethanol solution is added into the mixed solution, so that the thickness of a hydration layer around colloidal particles consisting of a plurality of tiny plant fibers, plant protein fragments, amino acids and the like in the mixed solution is damaged, the aim of breaking the stability of colloids is fulfilled, the clear and transparent fresh black tiger leaf extracting solution is better obtained, and the application of the clear and transparent fresh black tiger leaf extracting solution in high-grade bath lotion or cosmetic raw materials is widened.
Detailed Description
The present invention is further illustrated by the following description of specific embodiments, which are not intended to limit the invention, and various modifications and improvements can be made by those skilled in the art based on the basic idea of the invention, but within the scope of the invention, without departing from the basic idea of the invention.
The following examples, in which specific conditions are not specified, were conducted under conventional conditions, and the reagents and apparatus used therefor, in which manufacturers are not specified, were all conventional products commercially available. The ultramicro filter membrane sterilization filter is produced by Shaoxing Haina membrane technology Limited of Shaoxing in Zhejiang, model is SY-1, the interception aperture is 0.2 mu m, and the actual aperture is 0.1 mu m due to the replacement of a filter element in the actual operation process.
Example 1
The preparation method of the fresh black tiger leaf extract in embodiment 1 comprises the following steps:
s1, collecting: selecting fresh black tiger leaves as raw materials, preferably collecting enough daily processing amount in the early morning according to a plan, and paying attention to protect the sustainable growth of black tiger plants, wherein a certain amount of fresh leaves are reserved for each Tasmann;
s2, disinfection and sterilization: cleaning, naturally air drying, placing fresh leaf of Kadsura coccinea in a sealed bag, and introducing ozone for 5 min;
s3, crushing and pulping: cutting sterilized fresh black tiger leaves, putting the cut fresh black tiger leaves into a fruit and vegetable wall breaking machine, adding purified water which is 2 times of the weight of the fresh black tiger leaves, starting the wall breaking machine to break the fresh black tiger leaves into pulp, controlling the starting time of a high-speed gear of the wall breaking machine, and keeping the time not to exceed 20 seconds each time so as to avoid generating local high temperature and causing loss of effective components, and obtaining the original pulp of the fresh black tiger leaves after breaking into the pulp;
s4, primary gel breaking: adding a complex enzyme accounting for 0.1 percent of the mass of the fresh black tiger leaf primary pulp for primary gel breaking, stirring, and carrying out enzymolysis reaction at 35 ℃ for 7 hours, wherein the complex enzyme is prepared from cellulase, pectinase and papain in a proportion of 2: 0.5: 0.5 of mass ratio; standing, and separating the supernatant and the lower layer of colloidal solution, wherein the supernatant is stored at 4-8 ℃ to obtain a primary extracting solution A;
s5, secondary gel breaking: taking the lower layer colloidal solution, adding probiotics for secondary gel breaking, wherein the added probiotics is 'Angel wine fruit wine special yeast' purchased from the market, the added probiotics accounts for 0.05% of the lower layer colloidal solution, stirring to obtain fermentation liquor, and the temperature of the fermentation tank is controlled at 20 ℃. The fermentation time is 3 days, and in order to promote the fermentation process to be more complete, a certain amount of white granulated sugar is added into the fermentation liquor on the next day after the fermentation is started, wherein the adding amount can be controlled to be about 0.3% of the total amount of the fermentation liquor; after the fermentation is finished, the viscosity of the colloidal solution is greatly reduced, and then the colloidal solution is filtered under a 200-mesh filter screen to obtain primary extracting solution B and a solid filter cake;
s6, alcohol extraction: grinding the solid filter cake obtained in the step S5, adding 1 time of 95% ethanol solution (volume fraction) for extraction, stirring at 30 deg.C for 2h, and filtering to obtain primary extractive solution C;
s7, third gel breaking: mixing the primary extractive solution A and B, adjusting pH to 6.5 with 0.05M citric acid or 0.05M sodium carbonate, adding the primary extractive solution C, stirring, standing to obtain fine precipitate, slowly precipitating to bottom, sucking supernatant, and removing the precipitate;
s8, ultramicro membrane filtration: and (5) performing ultramicro membrane filtration on the supernatant obtained in the step S7 by using an ultramicro membrane sterilization filter to obtain the fresh black tiger leaf extracting solution.
The facial cleanser containing the fresh black tiger leaf extracting solution in the embodiment 1 comprises the following components in parts by weight: 15 parts of fresh black tiger leaf extract, 20 parts of deionized water, 3 parts of cocamidopropyl betaine, 4 parts of sodium cocoyl glycinate, 10 parts of glycerol, 25 parts of sodium methyl cocoyl taurate, 1 part of PEG-250 distearate, 1.5 parts of sodium chloride, 0.03 part of disodium EDTA, 0.05 part of aloe extract, 0.3 part of caprylyl hydroximic acid, 0.2 part of glyceryl caprylate, 0.1 part of propylene glycol and 0.05 part of essence for florescence.
The preparation method of the facial cleanser containing the fresh black tiger leaf extract in the embodiment 1 comprises the following steps:
a1, mixing deionized water, cocamidopropyl betaine, sodium cocoyl glycinate, glycerol, sodium methyl cocoyl taurate and EDTA disodium according to the formula ratio, and stirring at 80 ℃ until the mixture is transparent;
a2, cooling to 60 ℃, adding PEG-250 distearate with the formula amount, and stirring uniformly;
a3, cooling to 50 ℃, adding a sodium chloride solution, and stirring; wherein the sodium chloride solution is a pre-dissolved saturated aqueous solution of sodium chloride;
a4, cooling to 45 ℃, adding the formula amount of the fresh black tiger leaf extract, the aloe extract, the essence, and the pre-dispersed caprylyl hydroximic acid, glyceryl caprylate and propylene glycol; stirring, cooling and standing to obtain the final product.
The spray containing the fresh black tiger leaf extract in example 1 is composed of the following components in parts by weight: 35 parts of fresh black tiger leaf extracting solution; 65 parts of purified water; the preparation method comprises the following steps: mixing and stirring evenly, and packaging with a10 ml spray bottle under a sterile environment to obtain the product.
Example 2
The preparation method of the fresh black tiger leaf extract in embodiment 2 comprises the following steps:
s1, collecting: selecting fresh black tiger leaves as raw materials, preferably collecting enough daily processing amount in the early morning according to a plan, and paying attention to protect the sustainable growth of black tiger plants, wherein a certain amount of fresh leaves are reserved for each Tasmann;
s2, disinfection and sterilization: cleaning, naturally air drying, placing fresh leaf of Kadsura coccinea in a sealed bag, and introducing ozone for 10 min;
s3, crushing and pulping: cutting sterilized fresh black tiger leaves, putting the cut fresh black tiger leaves into a fruit and vegetable wall breaking machine, adding purified water which is 1 time of the weight of the fresh black tiger leaves, starting the wall breaking machine to break the fresh black tiger leaves into pulp, controlling the starting time of a high-speed gear of the wall breaking machine, and keeping the time not to exceed 20 seconds each time so as to avoid generating local high temperature and causing loss of effective components, and obtaining the original pulp of the fresh black tiger leaves after breaking into the pulp;
s4, primary gel breaking: adding a complex enzyme accounting for 0.3 percent of the mass of the fresh black tiger leaf primary pulp for primary gel breaking, stirring, and carrying out enzymolysis reaction at 38 ℃ for 3 hours, wherein the complex enzyme is prepared from cellulase, pectinase and papain in a proportion of 1: 1: 1 in a mass ratio; standing, and separating the supernatant and the lower layer of colloidal solution, wherein the supernatant is stored at 4-8 ℃ to obtain a primary extracting solution A;
s5, secondary gel breaking: taking the lower layer colloidal solution, adding probiotics for secondary gel breaking, wherein the added probiotics is 'Angel grape wine special yeast' purchased from the market, the added probiotics accounts for 0.2% of the lower layer colloidal solution, stirring to obtain fermentation liquor, and the temperature of the fermentation tank is controlled at 20 ℃. The fermentation time is 7 days, and in order to promote the fermentation process to be more complete, a certain amount of white granulated sugar can be added into the fermentation liquor the next day after the fermentation is started, wherein the added amount is controlled to be about 0.5 percent of the total amount of the fermentation liquor; after the fermentation is finished, the viscosity of the colloidal solution is greatly reduced, and then the colloidal solution is filtered under a 200-mesh filter screen to obtain primary extracting solution B and a solid filter cake;
s6, alcohol extraction: grinding the solid filter cake obtained in the step S5, adding 2 times of 95% ethanol solution by weight for extraction, stirring for 1h at 35 ℃, and filtering to obtain primary extracting solution C;
s7, third gel breaking: mixing the primary extractive solution A and B, adjusting pH to 7.5 with 0.05M citric acid or 0.05M sodium carbonate, adding the primary extractive solution C, stirring, standing to obtain fine precipitate, slowly precipitating to bottom, sucking supernatant, and removing the precipitate;
s8, ultramicro membrane filtration: and (5) performing ultramicro membrane filtration on the supernatant obtained in the step S7 by using an ultramicro membrane sterilization filter to obtain the fresh black tiger leaf extracting solution.
The facial cleanser with the fresh black tiger leaf extracting solution in the embodiment 2 comprises the following components in parts by weight: 30 parts of fresh black tiger leaf extract, 25 parts of deionized water, 5 parts of cocamidopropyl betaine, 2 parts of sodium cocoyl glycinate, 8 parts of glycerol, 30 parts of sodium methyl cocoyl taurate, 1.5 parts of PEG-250 distearate, 2 parts of sodium chloride, 0.05 part of EDTA disodium, 0.1 part of witch hazel extract, 0.5 part of caprylyl hydroximic acid, 0.3 part of glyceryl caprylate, 0.2 part of propylene glycol and 0.1 part of florist.
The preparation method of the facial cleanser containing the fresh black tiger leaf extract in the embodiment 2 comprises the following steps:
a1, mixing deionized water, cocamidopropyl betaine, sodium cocoyl glycinate, glycerol, sodium methyl cocoyl taurate and EDTA disodium according to the formula ratio, and stirring at 85 ℃ until the mixture is transparent;
a2, cooling to 60 ℃, adding PEG-250 distearate with the formula amount, and stirring uniformly;
a3, cooling to 50 ℃, adding a sodium chloride solution, and stirring; wherein the sodium chloride solution is a pre-dissolved saturated aqueous solution of sodium chloride;
a4, cooling to 45 ℃, and adding the formula amount of the fresh black tiger leaf extract, the witch hazel extract, the essence, and the dispersed caprylyl hydroximic acid, glyceryl caprylate and propylene glycol; stirring, cooling and standing to obtain the final product.
The spray containing the fresh black tiger leaf extract in example 2 is composed of the following components in parts by weight: 35 parts of fresh black tiger leaf extracting solution; 65 parts of purified water; the preparation method comprises the following steps: mixing and stirring evenly, and packaging with a10 ml spray bottle under a sterile environment to obtain the product.
Example 3
The preparation method of the fresh black tiger leaf extract in embodiment 3 comprises the following steps:
s1, collecting: selecting fresh black tiger leaves as raw materials, preferably collecting enough daily processing amount in the early morning according to a plan, and paying attention to protect the sustainable growth of black tiger plants, wherein a certain amount of fresh leaves are reserved for each Tasmann;
s2, disinfection and sterilization: cleaning, naturally air drying, placing fresh leaf of Kadsura coccinea in a sealed bag, and introducing ozone for 8 min;
s3, crushing and pulping: cutting sterilized fresh black tiger leaves, putting the cut fresh black tiger leaves into a fruit and vegetable wall breaking machine, adding purified water which is 1.5 times of the weight of the fresh black tiger leaves, starting the wall breaking machine to break the fresh black tiger leaves into pulp, controlling the starting time of the high-speed gear of the wall breaking machine to be not more than 20 seconds each time so as to avoid generating local high temperature to cause loss of effective components, and breaking the pulp to obtain the original pulp of the fresh black tiger leaves;
s4, primary gel breaking: adding a complex enzyme accounting for 0.2 percent of the mass of the fresh black tiger leaf primary pulp for primary gel breaking, stirring, and carrying out enzymolysis reaction at 35 ℃ for 7 hours, wherein the complex enzyme is prepared from cellulase, pectinase and papain in a proportion of 2: 1: 1 in a mass ratio; standing, and separating the supernatant and the lower layer of colloidal solution, wherein the supernatant is stored at 4-8 ℃ to obtain a primary extracting solution A;
s5, secondary gel breaking: taking the lower layer colloidal solution, adding probiotics for secondary gel breaking, wherein the added probiotics is 'Angel wine and fruit wine special yeast' purchased from the market, the added probiotics accounts for 0.12% of the lower layer colloidal solution, stirring to obtain fermentation liquor, and the temperature of the fermentation tank is controlled at 20 ℃. The fermentation time is 7 days, and in order to promote the fermentation process to be more complete, a certain amount of white granulated sugar is added into the fermentation liquor on the next day after the fermentation is started, wherein the adding amount can be controlled to be about 0.3% of the total amount of the fermentation liquor; after the fermentation is finished, the viscosity of the colloidal solution is greatly reduced, and then the colloidal solution can be filtered under a 200-mesh filter screen to obtain primary extracting solution B and a solid filter cake;
s6, alcohol extraction: grinding the solid filter cake obtained in the step S5, adding 2 times of 95% ethanol solution by weight for extraction, stirring for 2h at 30 ℃, and filtering to obtain primary extracting solution C;
s7, third gel breaking: mixing the primary extractive solution A and B, adjusting pH to 6.5 with 0.05M citric acid or 0.05M sodium carbonate, adding the primary extractive solution C, stirring, standing to obtain fine precipitate, slowly precipitating to bottom, sucking supernatant, and removing the precipitate;
s8, ultramicro membrane filtration: and (5) performing ultramicro membrane filtration on the supernatant obtained in the step S7 by using an ultramicro membrane sterilization filter to obtain the fresh black tiger leaf extracting solution.
The facial cleanser with the fresh black tiger leaf extracting solution in the embodiment 3 comprises the following components in parts by weight: 20 parts of fresh black tiger leaf extract, 30 parts of deionized water, 4 parts of cocamidopropyl betaine, 4 parts of sodium cocoyl glycinate, 8 parts of glycerol, 30 parts of sodium methyl cocoyl taurate, 1.5 parts of PEG-250 distearate, 2 parts of sodium chloride, 0.05 part of EDTA disodium, 0.1 part of witch hazel extract, 0.4 part of caprylyl hydroximic acid, 0.25 part of glyceryl caprylate, 0.15 part of propylene glycol and 0.05 part of florist.
The preparation method of the facial cleanser containing the fresh black tiger leaf extract in the embodiment 3 comprises the following steps:
a1, mixing deionized water, cocamidopropyl betaine, sodium cocoyl glycinate, glycerol, sodium methyl cocoyl taurate and EDTA disodium according to the formula ratio, and stirring at 80 ℃ until the mixture is transparent;
a2, cooling to 60 ℃, adding PEG-250 distearate with the formula amount, and stirring uniformly;
a3, cooling to 50 ℃, adding a sodium chloride solution, and stirring; wherein the sodium chloride solution is a pre-dissolved saturated aqueous solution of sodium chloride;
a4, cooling to 45 ℃, and adding the formula amount of the fresh black tiger leaf extract, the witch hazel extract, the essence, and the dispersed caprylyl hydroximic acid, glyceryl caprylate and propylene glycol; stirring, cooling and standing to obtain the final product.
The spray containing the fresh black tiger leaf extract in example 3 is composed of the following components in parts by weight: 35 parts of fresh black tiger leaf extracting solution; 65 parts of purified water; the preparation method comprises the following steps: mixing and stirring evenly, and packaging with a10 ml spray bottle under a sterile environment to obtain the product.
Comparative example 1
The preparation method of the fresh black tiger leaf extracting solution in the comparative example 1 comprises the following steps of:
s1, collecting: selecting fresh black tiger leaves as raw materials, preferably collecting enough daily processing amount in the early morning according to a plan, and paying attention to protect the sustainable growth of black tiger plants, wherein a certain amount of fresh leaves are reserved for each Tasmann;
s2, disinfection and sterilization: cleaning, naturally air drying, placing fresh leaf of Kadsura coccinea in a sealed bag, and introducing ozone for 8 min;
s3, crushing and pulping: cutting sterilized fresh black tiger leaves, putting the cut fresh black tiger leaves into a fruit and vegetable wall breaking machine, adding purified water which is 1.5 times of the weight of the fresh black tiger leaves, starting the wall breaking machine to break the fresh black tiger leaves into pulp, controlling the starting time of the high-speed gear of the wall breaking machine to be not more than 20 seconds each time so as to avoid generating local high temperature to cause loss of effective components, and breaking the pulp to obtain the original pulp of the fresh black tiger leaves;
s4, filtering by a filter screen: filtering with 600 mesh filter screen to obtain the fresh black tiger leaf extract of comparative example 1.
The facial cleanser with the fresh black tiger leaf extract in the comparative example 1 and the preparation method thereof are the same as those in the example 3.
Comparative example 2
The preparation method of the fresh black tiger leaf extract of the comparative example 2 comprises the following steps:
s1, collecting: selecting fresh black tiger leaves as raw materials, preferably collecting enough daily processing amount in the early morning according to a plan, and paying attention to protect the sustainable growth of black tiger plants, wherein a certain amount of fresh leaves are reserved for each Tasmann;
s2, disinfection and sterilization: cleaning, naturally air drying, placing fresh leaf of Kadsura coccinea in a sealed bag, and introducing ozone for 8 min;
s3, crushing and pulping: cutting sterilized fresh black tiger leaves, putting the cut fresh black tiger leaves into a fruit and vegetable wall breaking machine, adding purified water which is 1.5 times of the weight of the fresh black tiger leaves, starting the wall breaking machine to break the fresh black tiger leaves into pulp, controlling the starting time of the high-speed gear of the wall breaking machine to be not more than 20 seconds each time so as to avoid generating local high temperature to cause loss of effective components, and breaking the pulp to obtain the original pulp of the fresh black tiger leaves;
s4, primary gel breaking: adding a complex enzyme accounting for 0.2 percent of the mass of the fresh black tiger leaf primary pulp for primary gel breaking, stirring, and carrying out enzymolysis reaction at 35 ℃ for 7 hours, wherein the complex enzyme is prepared from cellulase, pectinase and papain in a proportion of 2: 1: 1 in a mass ratio; standing, and separating the supernatant and the lower layer of colloidal solution, wherein the supernatant is stored at 4-8 ℃ to obtain a primary extracting solution A;
s5, alcohol extraction: taking the lower layer colloidal solution in the step S4, adding 2 times of 95% ethanol solution by weight for extraction, stirring for 2h at 30 ℃, and filtering to obtain primary extracting solution C;
s6, secondary gel breaking: adjusting pH of the primary extractive solution A to 6.5 with 0.05M citric acid or 0.05M sodium carbonate, adding the primary extractive solution C, stirring, standing, sucking out supernatant, and removing bottom precipitate;
s7, ultramicro membrane filtration: and (4) filtering the supernatant obtained in the step (S6) by using a 0.1 mu ultrafiltration membrane to obtain the fresh black tiger leaf extracting solution of the comparative example 2.
The facial cleanser containing the fresh black tiger leaf extract and the preparation method thereof as well as the spray containing the fresh black tiger leaf extract and the preparation method thereof in the comparative example 2 are the same as those in the example 3.
Comparative example 3
The preparation method of the fresh black tiger leaf extracting solution in the comparative example 3 comprises the following steps of:
s1, collecting: selecting fresh black tiger leaves as raw materials, preferably collecting enough daily processing amount in the early morning according to a plan, and paying attention to protect the sustainable growth of black tiger plants, wherein a certain amount of fresh leaves are reserved for each Tasmann;
s2, disinfection and sterilization: cleaning, naturally air drying, placing fresh leaf of Kadsura coccinea in a sealed bag, and introducing ozone for 8 min;
s3, crushing and pulping: cutting sterilized fresh black tiger leaves, putting the cut fresh black tiger leaves into a fruit and vegetable wall breaking machine, adding purified water which is 1.5 times of the weight of the fresh black tiger leaves, starting the wall breaking machine to break the fresh black tiger leaves into pulp, controlling the starting time of the high-speed gear of the wall breaking machine to be not more than 20 seconds each time so as to avoid generating local high temperature to cause loss of effective components, and breaking the pulp to obtain the original pulp of the fresh black tiger leaves;
s4, primary gel breaking: adding a complex enzyme accounting for 0.2 percent of the mass of the fresh black tiger leaf primary pulp for primary gel breaking, stirring, and carrying out enzymolysis reaction at 35 ℃ for 7 hours, wherein the complex enzyme is prepared from cellulase, pectinase and papain in a proportion of 2: 1: 1 in a mass ratio; standing, and separating the supernatant and the lower layer of colloidal solution, wherein the supernatant is stored at 4-8 ℃ to obtain a primary extracting solution A;
s5, secondary gel breaking: taking the lower-layer colloidal solution, adding probiotics for secondary gel breaking, wherein the added probiotics are 'Angel wine and fruit wine special yeast' purchased from the market, the added probiotics account for 0.12 percent of the mass of the lower-layer colloidal solution, stirring is carried out to obtain fermentation liquor, the temperature of the fermentation tank is controlled at 20 ℃, the fermentation time is 7 days, and in order to promote the fermentation process to be more complete, a certain amount of white granulated sugar is added into the fermentation liquor in the next day after the fermentation is started, and the adding amount can be controlled to be about 1 percent of the total amount of the fermentation liquor; after the fermentation is finished, the viscosity of the colloidal solution is greatly reduced, and then the colloidal solution can be filtered under a 200-mesh filter screen to obtain primary extracting solution B and a solid filter cake, and the solid filter cake is discarded;
s6, third gel breaking: mixing the primary extractive solution A and B, adjusting pH to 6.5 with 0.05M citric acid or 0.05M sodium carbonate, standing, sucking out supernatant, and removing bottom precipitate;
s8, ultramicro membrane filtration: and (5) taking the supernatant obtained in the step S6 to obtain the fresh black tiger leaf extracting solution of the comparative example 3.
The facial cleanser containing the fresh black tiger leaf extract and the preparation method thereof as well as the spray containing the fresh black tiger leaf extract and the preparation method thereof in the comparative example 3 are the same as those in the example 3.
Comparative example 4
Comparative example 4 the operating condition parameters for preparing the fresh black tiger leaf extract, the facial cleanser containing the fresh black tiger leaf extract and the preparation method thereof, and the spray containing the fresh black tiger leaf extract and the preparation method thereof are the same as those in example 3 except that in the primary gel breaking process step, only 0.3 mass percent of cellulase is used as a single enzyme for the enzymolysis reaction, and no complex enzyme (cellulase, pectinase and papain are in a ratio of 2: 1: 1) is used for the enzymolysis reaction.
Test example 1 evaluation of appearance of Tiger extract liquid obtained by different extraction Processes
The evaluation and test method comprises the following steps of taking 50m L of the black tiger extract prepared in examples 1 to 3 and comparative example 1, placing the black tiger extract into a 100m L transparent colorimetric tube, then covering a stopper, placing the colorimetric tube into an oscillator, oscillating the colorimetric tube at 20 +/-0.5 ℃ for 5min, taking out the colorimetric tube, standing the colorimetric tube for 10min, measuring the viscosity of the colorimetric tube at the temperature of 20 +/-0.5 ℃ by using a rotary viscometer and recording the reading, repeating the measurement three times, expressing the result by using a mean value and expressing the viscosity unit by using centipoise (cP), standing the colorimetric tube for 2h, and observing and recording the precipitation generation state at the bottom of the colorimetric tube filled with the extract by using naked eyes and the clarity degree of the extract, wherein the experimental results are shown in Table 1:
TABLE 1 evaluation of appearance of Tiger extract obtained by different processes
From the results in table 1, the extracted solution of the fresh black tiger leaves prepared by the method has the viscosity of 1.19-1.23cP, lower viscosity and better fluidity; and the prepared extracting solution is clear, does not generate precipitates or floccules, and can meet the basic requirements of being used as cosmetic raw materials, wherein the embodiment 3 is the best embodiment of the invention.
The fresh black tiger leaf extracting solution in the comparative example 1 is prepared by directly filtering after crushing and pulping, and compared with the fresh black tiger leaf extracting solution in the example 3 of the invention, the fresh black tiger leaf extracting solution prepared in the comparative example 1 is very turbid, a large amount of sticky colloid blocks a filter screen during filtering, and after the obtained fresh black tiger leaf extracting solution is placed still, the extracting solution in a colorimetric tube is in a suspension state, and a large amount of turbidity appears at the bottom.
Test example 2 Effect of the extract solution of Kadsura coccinea of the present invention on moisture, pH, melanin and hemoglobin of mouse skin
Taking 100 SPF female mice with the weight of 20 +/-2 g, randomly dividing the mice into 10 groups, wherein each group comprises 10 mice, 8 groups are test groups, 1 group is a model group, and 1 group is a blank control group, shearing off coarse hairs on the backs of the mice by using scissors, then removing the rest fine hairs cleanly by using a shaver to ensure that the back skins are fully exposed, the area of the shaved hairs is 3CM × CM, depilating for 1 time every week, and cleaning the depilated hairs by using warm water after depilating, in the experimental process, respectively regularly coating the fresh black tiger leaf extracting solution of examples 1-3 and comparative examples 1-4 on the backs of the mice, coating the Skin which is uniform in thickness and can cover the exposed backs of the mice, placing the coated back experimental parts under an SS-04B type ultraviolet light therapeutic apparatus for irradiating for 10min, irradiating for 40CM for once every day, continuously irradiating for two weeks, directly irradiating the model groups for 10min under the ultraviolet light, not performing any water content measurement on the blank groups, also performing the Skin pH value measurement by using an ultraviolet light, respectively performing a pH value measurement on a melanin light instrument, a Skin measuring probe for the Skin of the mice, a rat, a melanin test group, and a probe for measuring the melanin test group (MCK-32), and a PH value of the mice, a probe for measuring the melanin test group, and a Skin test probe for measuring a melanin test group (MCK-19), and a test result of the mice, a melanin test probe for measuring a melanin test group, a test probe for measuring a melanin test group for measuring a melanin test probe for measuring a melanin test group, a melanin test probe for measuring a
It is shown that,
the average of the results of 10 tests in each group is shown, s is the standard deviation, where P is<0.05 is statistically significant, and the results are shown in Table 1:
TABLE 2 Effect of the Tilapia saxifraga leaf extract of the present invention on moisture, pH, melanin and heme of mouse skin
Comparison of notes with blank controls*P<0.05
From the test results in table 2, it can be seen that, compared with the model group, the fresh black tiger leaf extract of the present invention has the advantages of increased moisture content and decreased pH value after being applied to the skin on the back of the mouse, which indicates that the fresh black tiger leaf extract of the present invention has good moisturizing effect and the melanin and heme values are lower than those of the model group, which indicates that the fresh black tiger leaf extract of the present invention can effectively inhibit the generation of melanin and heme in the skin under stress environment.
Compared with the example 3, the fresh black tiger leaf extracting solution of the comparative example 1 is prepared by directly filtering after crushing and pulping, and the results in the table 2 show that under the irradiation of an ultraviolet phototherapy lamp, although the moisture value of the back skin of a mouse is higher than that of a blank control group, the moisture value is obviously lower than that of the example 3, the deposition of melanin and heme is greater than that of the example 3, which indicates that most of effective components for inhibiting pigments (whitening and freckle removing) in the fresh black tiger leaf extracting solution obtained by directly crushing and filtering are lost, so the effects of inhibiting the generation and moistening of the pigments are greatly reduced, mainly because the viscosity of the solution obtained by directly crushing and filtering the fresh black tiger leaves is very high, and most of the effective components are wrapped by the sticky jelly, so that the effective components are lost.
And (3) after the fresh black tiger leaf extracting solution of the comparative example 2 is subjected to primary gel breaking and enzymolysis, filtering to obtain a lower-layer colloidal solution, fermenting without adding probiotics, directly performing alcohol extraction on the lower-layer colloidal solution, filtering, and combining filtrates to obtain the fresh black tiger leaf extracting solution of the comparative example 2. The prepared fresh black tiger leaf extracting solution has reduced pigment inhibiting capacity, and the moisture content of the skin on the back of a mouse is correspondingly reduced, probably because a probiotic fermentation step is lacked, various enzyme essences generated in the fermentation process are reduced, and the enzymes have certain effects on whitening, moistening and removing melanin of the skin.
The fresh black cutworm leaf extracting solution of the comparative example 3 is not subjected to the alcohol extraction step, and compared with the example 3 of the invention, the viscosity of the extracting solution of the comparative example 3 is obviously higher than that of the example 3 because 2 times of ethanol solution with the content of 95% by weight needs to be added in the alcohol extraction process. It can be seen from the experimental data in table 2 that the pigment removing performance is inferior to that of example 3, which is probably because the effective components in the finally obtained extract of the fresh black tiger leaves are reduced because the ethanol solvent is not added in comparative example 3 for extraction, and the effective components for inhibiting the pigment coated on the back of the mouse with the same area are correspondingly reduced, thereby obtaining the experimental result.
In the primary gel breaking process step of the fresh black tiger leaf extract in the comparative example 4, only 0.3 mass percent of cellulase is used as single enzyme for enzymolysis reaction, and no complex enzyme (the mass ratio of cellulase, pectinase and papain is 2: 1: 1) is used for enzymolysis reaction, so that the effect of inhibiting the pigment is poorer than that of the example 3, because the complex enzyme can be used for sufficiently hydrolyzing the original pulp of the fresh black tiger leaves, and more effective components capable of inhibiting the pigment and whitening are obtained.
Test example 3 evaluation test of the Performance of facial cleanser and spray containing the extract solution of Tiger fresh leaves according to the present invention
The performance evaluation method comprises the following steps: 60 subjects of different ages, with significantly dry skin, dark color, some mottling or pigmentation, were selected and tested for one month. The 60 subjects were divided into two groups, one group being the test group and one group being the control group. The test group is that half of the test subjects use facial cleanser containing the extract of the fresh black tiger leaves and are matched with a small bottle (10 ml) of spray containing the extract of the fresh black tiger leaves (the facial cleanser and the spray used by the test group are prepared according to the proportion and the method of the invention in the embodiment 3, both the facial cleanser and the spray contain the extract of the fresh black tiger leaves), and the face is sprayed with the spray after the facial cleanser is used for cleaning the face; the other half of the test subjects served as control groups (the facial cleanser and the spray of the control group were prepared by the formulation and preparation method of the invention in example 3, but the extracted solution of the fresh black tiger leaves was not added in the formulation, and the rest was the same), and were used 5 days per week with a test period of 4 weeks, and the effect of each test subject was carefully observed, and whether there was any adverse effect or adverse reaction was noticed.
The evaluation standard of curative effect is as follows: the effect is shown: after the facial cleanser and the spray are used for 4 weeks, the color spots obviously fade, the skin color is brightened and is not dark yellow any more, and compared with the prior art, the skin becomes tender and glossy, and wrinkles become light;
the method has the following advantages: after the facial cleanser and the spray are used for 4 weeks, color spots are faded, the skin color is brightened, and compared with the prior art, the skin becomes glossier and wrinkles become lighter;
and (4) invalidation: after 4 weeks, the color spots of the facial cleanser and the spray are not obviously changed, and the skin is still dry, dark yellow and dull.
TABLE 3 evaluation test of the performance of facial cleanser and spray containing the extract of fresh black tiger leaves of the present invention
As can be seen from the data in Table 3, the total effective rate of the test subjects using the Tiger fresh leaf extract facial cleanser and the spray for 4 weeks is far higher than that of the control group. Evaluation test results can prove that the facial cleanser containing the fresh black tiger leaf extracting solution and the spray have various effects of moisturizing, whitening, brightening, removing freckles and the like when being used in a matching way, and no side effect or adverse reaction is found after observation, so that the facial cleanser can be used for daily skin care.
It will be appreciated by those skilled in the art that the above embodiments are merely illustrative of the principles and utilities of the present invention and are not intended to limit the invention. Any person skilled in the art can modify or change the above-mentioned embodiments without departing from the spirit and scope of the present invention. Accordingly, it is intended that all equivalent modifications or changes which can be made by those skilled in the art without departing from the spirit and technical spirit of the present invention be covered by the claims of the present invention.
Claims (10)
1. A preparation method of a fresh black tiger leaf extracting solution is characterized by comprising the following steps:
s1, collecting: selecting fresh black tiger leaves as a raw material;
s2, disinfection and sterilization: cleaning, naturally drying, and putting the fresh black tiger leaves into a sealed bag and introducing ozone for 5-10 min;
s3, crushing and pulping: chopping the sterilized fresh black tiger leaves, putting into a wall breaking machine, adding water, and crushing into pulp to obtain the original pulp of the fresh black tiger leaves;
s4, primary gel breaking: adding a complex enzyme for primary gel breaking, stirring, performing enzymolysis reaction at 35-38 ℃, reacting for 3-7 h, standing, and separating supernatant and lower-layer colloidal solution, wherein the supernatant is stored at 4-8 ℃ to obtain primary extract A;
s5, secondary gel breaking: taking the lower-layer colloidal solution, adding probiotics, stirring to obtain a fermentation liquid, fermenting for 3-7 days at 20 ℃, and filtering to obtain a primary extracting solution B and a solid filter cake;
s6, alcohol extraction: crushing the solid filter cake obtained in the step S5, adding 95% ethanol solution for extraction, stirring for 1-2 h at 30-35 ℃, and filtering to obtain primary extracting solution C;
s7, third gel breaking: mixing the primary extracting solution A and the primary extracting solution B, adjusting the pH value to 6.5-7.5, adding the primary extracting solution C, stirring, standing, and taking supernatant after precipitation;
s8, ultramicro membrane filtration: and (5) carrying out ultramicro membrane filtration on the supernatant obtained in the step S7 to obtain a fresh black tiger leaf extracting solution.
2. The method for preparing the extracting solution of the fresh black tiger leaves as claimed in claim 1, wherein in the step S4, the mass of the compound enzyme is 0.1-0.3% of the mass of the fresh black tiger leaves, and the compound enzyme is prepared from cellulose, pectinase and papain in a ratio of 2: 0.5-2: 0.5-2 mass ratio.
3. The method for preparing the fresh black tiger leaf extracting solution according to claim 1, wherein in the step S5, the probiotics are selected from special Anqi wine and wine yeast, and the mass of the probiotics is 0.05-0.2% of the mass of the lower layer colloid solution.
4. The method for preparing the fresh black tiger leaf extract as claimed in claim 1, wherein in the step S5, white granulated sugar is added into the fermentation liquor the next day after the fermentation is started, and the addition amount of the white granulated sugar is 0.2-0.5% of the total weight of the fermentation liquor.
5. The method of preparing the extracted solution of saxifraga stolonifera leaves as claimed in claim 1, wherein the weight ratio of the solid filter cake to the 95% ethanol solution in step S6 is 1: 1 to 2.
6. The extracted solution of fresh black tiger leaves obtained by the method for preparing the extracted solution of fresh black tiger leaves according to any one of claims 1 to 5.
7. The use of the fresh black tiger leaf extract in the preparation of cosmetics with whitening and freckle removing effects according to claim 6, wherein the cosmetics comprise paste, emulsion, film, spray, gel or soap.
8. A facial cleanser containing the fresh black tiger leaf extracting solution of claim 6 is characterized by comprising the following components in parts by weight: 15-30 parts of fresh black tiger leaf extracting solution, 20-25 parts of deionized water, 3-5 parts of cocamidopropyl betaine, 2-4 parts of sodium cocoyl glycinate, 8-10 parts of glycerol, 25-30 parts of sodium methyl cocoyl taurate, 1-1.5 parts of PEG-250 distearate, 1.5-2 parts of sodium chloride, 0.03-0.05 part of disodium EDTA, 0.05-0.1 part of soothing and moisturizing extracting solution, 0.3-0.5 part of caprylyl hydroximic acid, 0.2-0.3 part of glyceryl caprylate, 0.1-0.2 part of propylene glycol and 0.05-0.1 part of essence.
9. The facial cleanser according to claim 8, wherein the soothing and moisturizing extracting solution is an aloe extracting solution or a witch hazel extracting solution.
10. The method for preparing the facial cleanser with the extract of fresh black tiger leaves as claimed in claim 8, comprising the following steps:
a1, mixing deionized water, cocamidopropyl betaine, sodium cocoyl glycinate, glycerol, sodium methyl cocoyl taurate and EDTA disodium according to the formula ratio, and stirring at 80-85 ℃ until the mixture is transparent;
a2, cooling to 60 ℃, adding PEG-250 distearate with the formula amount, and stirring uniformly;
a3, cooling to 50 ℃, adding a sodium chloride solution, and stirring; wherein the sodium chloride solution is a pre-dissolved saturated aqueous solution of sodium chloride;
a4, cooling to 45 ℃, adding the formula amount of the fresh black tiger leaf extract, the soothing and moisturizing extract, the essence, and the pre-dispersed caprylyl hydroximic acid, glyceryl caprylate and propylene glycol; stirring, cooling and standing to obtain the final product.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113024683A (en) * | 2021-03-18 | 2021-06-25 | 广西壮族自治区药用植物园 | Black tiger stem and leaf polysaccharide and application thereof |
| CN114042020A (en) * | 2021-10-09 | 2022-02-15 | 湖南医药学院 | Black tiger mask essence and preparation method and application thereof |
| CN114259444A (en) * | 2022-01-18 | 2022-04-01 | 湖南环境生物职业技术学院 | A Tiger fruit extract with whitening effect, its preparation method and application in preparing bath lotion with whitening effect |
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2020
- 2020-05-08 CN CN202010382906.XA patent/CN111419760A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113024683A (en) * | 2021-03-18 | 2021-06-25 | 广西壮族自治区药用植物园 | Black tiger stem and leaf polysaccharide and application thereof |
| CN113024683B (en) * | 2021-03-18 | 2022-08-19 | 广西壮族自治区药用植物园 | Black tiger stem and leaf polysaccharide and application thereof |
| CN114042020A (en) * | 2021-10-09 | 2022-02-15 | 湖南医药学院 | Black tiger mask essence and preparation method and application thereof |
| CN114259444A (en) * | 2022-01-18 | 2022-04-01 | 湖南环境生物职业技术学院 | A Tiger fruit extract with whitening effect, its preparation method and application in preparing bath lotion with whitening effect |
| CN114259444B (en) * | 2022-01-18 | 2023-06-02 | 湖南环境生物职业技术学院 | A black tiger fruit extract with whitening effect, its preparation method and application in preparing bath lotion with whitening effect |
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