CN110317685B

CN110317685B - Aronia melanocarpa perfumed soap

Info

Publication number: CN110317685B
Application number: CN201910658706.XA
Authority: CN
Inventors: 辛广; 陈世富; 王健
Original assignee: Liaoning Fukangyuan Black Fruit Of Sorbus Technology Development Co ltd
Current assignee: Liaoning Fukangyuan Black Fruit Of Sorbus Technology Development Co ltd
Priority date: 2019-07-22
Filing date: 2019-07-22
Publication date: 2021-03-16
Anticipated expiration: 2039-07-22
Also published as: CN110317685A

Abstract

The invention provides aronia melanocarpa perfumed soap, which belongs to the field of washing and skin care products, and the preparation method comprises the following steps: providing an aronia melanocarpa extract; providing an acidic environment and dispersing the extract in a protective colloid to form micelles; providing an external water phase, and dispersing the micelle in the external water phase to obtain a multiple emulsion; providing a soap base, mixing the multiple emulsion with the soap base, and molding to obtain the perfumed soap; the protective colloid is pectin, and no surfactant is added into the soap. The perfumed soap disclosed by the invention has the color and the fragrance of aronia melanocarpa, is strong in antibacterial and mosquito-repellent capacity, high in transparency of a soap body, fine and smooth in foam, and non-dry and tense after use, and has the health care, nursing and beautifying effects of relieving skin allergy and preventing scars from being formed when wounds are healed; the preparation method can improve the stability and compatibility of the soap body, inhibit high-temperature degradation and oxidative rancidity in the soap body, prevent cracking and discoloration, prevent calcium and magnesium soaps from coagulating and reducing the viscosity in washing, reduce skin irritation without adding a surfactant, and save the using amount of auxiliary materials.

Description

Aronia melanocarpa perfumed soap

Technical Field

The invention belongs to the field of washing and skin care products, and particularly relates to aronia melanocarpa perfumed soap.

Background

In the industry of personal cleaning products, the perfumed soap is deeply favored by consumers due to the advantages of strong functionality, convenient use and carrying, low price, multiple varieties and the like. The main function of the soap is to remove the surface dirt of the human body, but with the improvement of the living standard of people and the personalized requirements of consumption behaviors, the common soap only with the dirt removing function can not meet the requirements of the public, the public has more and higher requirements on the quality and the color variety of the soap product, a single soap variety is difficult to occupy the market, and some novel soaps, such as transparent soaps, whitening soaps, compound soaps, functional soaps and the like, become a new favorite of consumers due to excellent application effect, but problems, such as cracking, non-durability, color change rancidity, unsmooth stripping and the like, easily occur in the soap production due to the addition of a plurality of elements, usually in the actual production, the effects of improving the quality and increasing the efficiency of the soap can be achieved by introducing anionic surfactants or nonionic surfactants and the like, but the surfactants have greater irritation to the skin, and the skin is easy to be excessively dry and tense after the soap is used, the sensory experience is slightly poor when the soap is used, so the production and preparation method and the raw material selection of the soap need to be intensively researched and developed.

Aronia melanocarpa, also called as aronia melanocarpa, contains various nutrient substances such as carotenoid, anthocyanin, procyanidine, tannic acid, pectin, organic acid, protein, L-ascorbic acid, flavone, chlorogenic acid, folic acid and the like, and has remarkable health care effect. The fresh Sorbus pohuashanensis fruit and its extract have special therapeutic effect on cardiovascular and cerebrovascular diseases such as heart disease and hypertension, and also have good therapeutic effect on radiation disease and heavy metal poisoning. The content of phenolic substances in the aronia melanocarpa fruit is the highest in known plants, the phenolic substances are important substances for improving the vascular structure and function, the circulatory system is improved, the antioxidant capacity is high, and the risks of cancers, blood coagulation and cardiovascular diseases can be effectively reduced; the anthocyanin has obvious effects on reducing blood fat, resisting cancer, delaying aging and the like. In addition, the Aronia melanocarpa fruit is rich in vitamins and antioxidants, and has the functions of removing chloasma and resisting aging.

In europe, aronia melanocarpa has been classified as a food with official authority of the european union. The research and development of the fruit on eating have made great progress, and various products such as fruit wine, fruit juice, fruit jelly powder and the like have been developed. There have been many studies in pharmaceutical applications, but they are still somewhat rare in washing skin care products. Based on the above, the aronia melanocarpa perfumed soap is developed and provided, not only has a decontamination effect, but also has a health care effect on a human body, and can increase market competitiveness.

Disclosure of Invention

The invention aims to provide the aronia melanocarpa soap which has strong antibacterial and mosquito repellent capacity, high soap transparency, fine foam, excellent concentration and fullness without adding industrial essence, can relieve skin allergy, prevent excessive proliferation of granulation tissues without forming scars when wounds heal, avoid the dry and tight sensory experience after use, has the special color of aronia melanocarpa and the skin health care and nursing and beautifying effects, can improve the stability and compatibility of the soap body, eliminate the phenomenon of low bonding rate of a D-shaped glycosyl extract and pectin, inhibit high-temperature degradation and oxidative rancidity in the soap body, prevent the soap body from cracking and changing color and deteriorating, prevent calcium magnesium soap coagulation in washing and reduce the viscosity of the calcium magnesium soap, and does not additionally add a surfactant component to reduce skin irritation, thereby saving the auxiliary material consumption and production cost.

The technical scheme adopted by the invention for realizing the purpose is as follows:

a preparation method of Aronia melanocarpa soap comprises providing Aronia melanocarpa extract; providing an acidic environment, and dispersing the aronia melanocarpa extract in a protective colloid to form micelles; providing an external water phase, and dispersing the micelle in the external water phase to obtain a multiple emulsion; providing a soap base, mixing the compound emulsion with the soap base, and molding to obtain the aronia melanocarpa perfumed soap;

the protective colloid is pectin, and no surfactant is added into the Aronia melanocarpa soap. The aronia melanocarpa soap prepared by the preparation method has the advantages of strong cleaning, stain removal, antibacterial and mosquito repellent capabilities, rich and fine foam, natural and full aroma, good stability and compatibility, no cracking, no deterioration and no discoloration during storage and use, capability of relieving skin allergy, promotion of skin wound healing and prevention of scar formation, skin care and beauty effect, and due to the fact that no surfactant component is additionally added to the soap, skin irritation is reduced, and sensory experience of dryness and tightness after use is avoided.

In an embodiment of the invention, the Aronia melanocarpa extract comprises 15-35wt% of an aqueous extract, 30-45wt% of an organic solvent extract and 5-20wt% of Aronia melanocarpa volatile oil. The aronia melanocarpa contains various substances with health care effects, can achieve the effects of diminishing inflammation, resisting bacteria, resisting oxidation, delaying aging and the like, extracts functional substances in fruits, can maximize the health care effect of the soap, avoids the loss of volatile substances, and saves the using amount of auxiliary materials.

In a more specific embodiment of the invention, the step of extracting the aqueous extract is: crushing and homogenizing the aronia melanocarpa fruits, adding double distilled water of which the amount is 5-8 times of that of the aronia melanocarpa fruits, extracting for 1-2 hours at the temperature of 60-85 ℃, centrifuging, taking filtrate, and concentrating to obtain paste, namely the aronia melanocarpa aqueous extract. The low-temperature extraction can avoid partial effective substances from losing the biological activity and the efficacy due to high-temperature oxidative deterioration.

In a more specific embodiment of the invention, the organic solvent extract is prepared under the extraction conditions: the feed-liquid ratio is 1:10-20(g/L), the pH is 2-4, the temperature is 50-60 ℃, and the time is 1.5-2.5 h. Under acidic environment, the interaction between cell wall and vacuole components in the pulp is weakened, so that the extraction rate and bioavailability of the solute can be improved, and the color characteristic and chemical stability of the solute are maintained. The organic solvent is an organic solvent commonly used in the extraction in the field, which is not described in detail herein, but preferably, the organic solvent is ethanol.

In a more specific embodiment of the invention, the aronia melanocarpa volatile oil is prepared by the following steps: the flow rate is 5-20m³Continuously washing the organic solvent extract with water vapor/min for 1-2 hr, collecting and condensing the gas, separating oil and water, and keeping the temperature of oil phase at 75-90 deg.C for 0.5-1 hr to obtain Aronia melanocarpa volatile oil. The volatile components can be separated and collected from the extracting solution by continuously washing with water vapor, so that the volatile oil escaping loss caused by the solvent removal of the extracting solution is avoided, the volatile oil can be collected and used in the soap to increase the fragrance and the health care effect, and the bioavailability is improved.

In an embodiment of the invention, micelles are made by the following process: dispersing Aronia melanocarpa extract in acidic environment with pH of 2.5-3.5, adding 45-60% pectin solution, magnetically stirring, and standing at 0-5 deg.C in dark for 10-12h to obtain micelle. The aronia melanocarpa extract and the pectin are combined to form micelles, so that the toilet soap is prevented from being discolored and deteriorated due to oxidative rancidity during the storage period and the using period, the rapid degradation of the extract at high temperature can be relieved or inhibited, the color and the health care effect of the toilet soap are protected, the shelf life of the toilet soap is prolonged, and the long-term health care effect of the toilet soap is maintained.

In an embodiment of the invention, the acidic environment is provided by a citric acid-sodium hydrogen phosphate buffer; the buffer solution also contains 0.1 to 0.5 weight percent of 2, 5-dipyridyl carboxylic acid and 0.05 to 0.2 weight percent of L-3-phenyllactic acid. Under the acidic environment, free carboxyl and hydroxyl in the system are subjected to ion crosslinking with positive cations, so that the binding effect of components such as anthocyanin and the like in the extract and pectin is enhanced, the stability of the extract is enhanced, 2, 5-dipicolinic acid and L-3-phenyllactic acid are added into the binding system, the hydrogen bonding effect can be preferentially generated with D-configuration xyloside in glycosyl groups contained in the extract, the binding effect is realized by the bridging effect so as to be combined with the pectin, the phenomenon that the binding rate of the extract with D-configuration glycosyl groups and the pectin is low is eliminated, the bioavailability is improved, on the other hand, the hydroxyl and the carboxyl can be combined with amino or amino acid residues of collagen to inhibit the proliferation of collagen cells, the expression level of Connective Tissue Growth Factors (CTGF) of fibers is reduced, the synthesis of the collagen fibers is further reduced, and granulation tissues can not excessively proliferate when skin wounds heal, scar formation is prevented.

In an embodiment of the invention, the multiple emulsion is prepared by the following method: dissolving polyvinyl alcohol to prepare an external water phase with the concentration of 1-3%, adding the external water phase into a micelle according to the weight ratio of 1:5-8, homogenizing at the rotation speed of 3000-. Pigment-containing substances such as anthocyanin in aronia melanocarpa exist stably in a red-yellow-melted salt cation form under an acidic environment, and once the external pH changes, anthocyanin molecules are easy to change in color, so that the color of the soap is influenced negatively, therefore, micelles are wrapped into an emulsion droplet form by using an external water phase, on one hand, the bioactivity of the soap can be protected, the deterioration of the soap can be prevented, on the other hand, the compatibility of the external water phase and a soap base is stronger, the compatibility between an extract and the components of the micelles and the soap base can be increased, and the soap body is prevented from cracking to generate cracks, so that the appearance and the aesthetic degree are influenced.

In an embodiment of the invention, the molding soap base is in a molten state; the soap base is melted by heating over water at 45-55 deg.C. The soap base is melted and then mixed with the multiple emulsion, so that the compatibility of the two substances can be improved, the components in the soap body can be uniformly dispersed, and the evaporation of water in a mixed system can be facilitated, so that the transparency of the soap body is improved, and the appearance is optimized.

In an embodiment of the invention, the external aqueous phase further comprises 3-10wt% of a repellent; the repellent is at least one of anophelifuge, lemongrass oil, oleum Menthae Dementholatum, and geranium oil. More preferably, the repellent is peppermint oil. Further, when the repellent is a mixture of two or more selected from the group consisting of 45-55% peppermint oil. The repellent has the effect of repelling mosquitoes, so that the soap has the effect of repelling mosquitoes, is long in repelling time and suitable for various skin conditions, and meanwhile, the components in the repellent can emit the fragrance of natural essential oil, so that the fragrance concentration and the fullness of the soap can be increased, and the addition of industrial essence can be avoided. Preferably, the peppermint oil component stimulates the nerve terminal receptors of the skin, generates a cooling feeling and enriches the sensory experience of the soap.

The invention also provides the aronia melanocarpa soap prepared by the preparation method, and the aronia melanocarpa soap comprises the following raw materials in parts by weight: 4-45 parts of aronia melanocarpa extract and 55-95 parts of soap base. The aronia melanocarpa perfumed soap has the special color and fragrance of aronia melanocarpa fruits, is high in transparency, has the effects of health care and skin care and beauty under the premise of keeping the cleaning effect, and remarkably improves the market competitiveness and the application prospect.

The invention has the beneficial effects that:

1) according to the invention, functional active ingredients in aronia melanocarpa are extracted in different modes, so that the health-care effect of the soap can be maximally improved, the bioavailability of raw materials is improved, the special color and fragrance of the active ingredients can be kept, the fragrance concentration and fullness of the soap are increased, and the addition of industrial essence can be avoided;

2) in the invention, the volatile oil is effectively collected by flushing the organic solvent extracting solution with water vapor, so that the volatile oil escape loss is avoided, the fragrance and the health care effect are enhanced when the volatile oil is used in the perfumed soap, and the using amount of auxiliary materials is saved;

3) according to the invention, the aronia melanocarpa extract is combined with pectin to form micelles, and then the micelles are coated with polyvinyl alcohol to form double emulsions, so that the stability and compatibility of the extract are improved, the phenomenon that the combination rate of the extract with D-configuration glycosyl is low is eliminated, the extract is not discolored and deteriorated due to oxidative rancidity, and the rapid degradation of the extract at high temperature can be relieved or inhibited, so that the color and the health care effect of the soap are protected, the soap is not cracked during storage and use, the healing of skin wounds can be promoted, the excessive proliferation of granulation tissues during the healing of the wounds is prevented, the formation of scars is avoided, and the skin care and beauty;

4) the soap provided by the invention has strong cleaning, antibacterial and mosquito repellent capabilities, high soap transparency and fine foam, can relieve skin allergy, can prevent coagulation of calcium-magnesium soap generated in washing, obviously reduces the viscosity of the calcium-magnesium soap, does not additionally add surfactant components, reduces skin irritation, avoids the dry and tight sensory experience after use, saves the auxiliary material consumption and production cost, has the health-care and skin-care beautifying effects on the premise of keeping the cleaning effect, and obviously improves the market competitiveness and application prospect.

The aronia melanocarpa perfumed soap provided by the invention adopts the technical scheme, overcomes the defects of the prior art, and is reasonable in design and convenient to operate.

Drawings

Fig. 1 is a pattern diagram of a product of aronia melanocarpa soap;

FIG. 2 is a schematic diagram showing the mosquito repellent effect test result of the aronia melanocarpa soap;

FIG. 3 is a schematic diagram showing the change in stability of an extract of aronia melanocarpa soap under high temperature storage conditions;

fig. 4 is a schematic diagram showing the effect of aronia melanocarpa soap on changes in CTGF immunohistochemical density values of wound area tissues.

Detailed Description

The technical solution of the present invention is further described in detail below with reference to the following detailed description and the accompanying drawings:

example 1:

a preparation method of Aronia melanocarpa soap comprises providing Aronia melanocarpa extract; providing an acidic environment, and dispersing the aronia melanocarpa extract in a protective colloid to form micelles; providing an external water phase, and dispersing the micelle in the external water phase to obtain a multiple emulsion; providing a soap base, mixing the compound emulsion with the soap base, and molding to obtain the aronia melanocarpa perfumed soap; the protective colloid is pectin, and no surfactant is added into the Aronia melanocarpa soap. The aronia melanocarpa soap prepared by the preparation method has the advantages of strong cleaning, stain removal, antibacterial and mosquito repellent capabilities, rich and fine foam, natural and full aroma, good stability and compatibility, no cracking, no deterioration and no discoloration during storage and use, capability of relieving skin allergy, promotion of skin wound healing and prevention of scar formation, skin care and beauty effect, and due to the fact that no surfactant component is additionally added to the soap, skin irritation is reduced, and sensory experience of dryness and tightness after use is avoided.

The Aronia melanocarpa extract comprises 25 wt% of an aqueous extract, 35wt% of an organic solvent extract and 10wt% of an Aronia melanocarpa volatile oil. The aronia melanocarpa contains various substances with health care effects, can achieve the effects of diminishing inflammation, resisting bacteria, resisting oxidation, delaying aging and the like, extracts functional substances in fruits, can maximize the health care effect of the soap, avoids the loss of volatile substances, and saves the using amount of auxiliary materials.

The extraction steps of the aqueous extract are as follows: crushing and homogenizing the aronia melanocarpa fruits, adding 5 times of double distilled water, extracting for 2 hours at the temperature of 65 ℃, centrifuging, taking filtrate, and concentrating to obtain paste, namely the aronia melanocarpa aqueous extract. The low-temperature extraction can avoid partial effective substances from losing the biological activity and the efficacy due to high-temperature oxidative deterioration.

The extraction conditions for the preparation of the organic solvent extract are as follows: the feed-liquid ratio is 1:12(g/L), the pH is 2.5, the temperature is 55 ℃, and the time is 2.5 h. Under acidic environment, the interaction between cell wall and vacuole components in the pulp is weakened, so that the extraction rate and bioavailability of the solute can be improved, and the color characteristic and chemical stability of the solute are maintained. The organic solvent is ethanol.

The aronia melanocarpa volatile oil is prepared by the following steps: the flow rate is 18m³Continuously washing the organic solvent extract for 1h with water vapor/min, collecting and condensing the gas escaping from washing, performing oil-water separation, and keeping the temperature of the oil phase at 80 ℃ for 1h to obtain the aronia melanocarpa volatile oil. The volatile components can be separated and collected from the extracting solution by continuously washing with water vapor, so that the volatile oil escape loss caused by solvent removal of the extracting solution is avoided, and the volatile oil can be collectedThe hair oil can be used in toilet soap for improving fragrance and health promotion, and is beneficial for improving bioavailability.

The micelle is prepared by the following method: dispersing Aronia melanocarpa extract in acidic environment with pH of 2.5, adding 60% pectin solution, magnetically stirring, and standing at 5 deg.C in dark place for 10 hr to obtain micelle. The aronia melanocarpa extract and the pectin are combined to form micelles, so that the toilet soap is prevented from being discolored and deteriorated due to oxidative rancidity during the storage period and the using period, the rapid degradation of the extract at high temperature can be relieved or inhibited, the color and the health care effect of the toilet soap are protected, the shelf life of the toilet soap is prolonged, and the long-term health care effect of the toilet soap is maintained.

The acidic environment is provided by a citric acid-sodium hydrogen phosphate buffer solution; the buffer solution also contains 0.25 wt% of 2, 5-dipyridyl carboxylic acid and 0.05 wt% of L-3-phenyllactic acid. Under the acidic environment, free carboxyl and hydroxyl in the system are subjected to ion crosslinking with positive cations, so that the binding effect of components such as anthocyanin and the like in the extract and pectin is enhanced, the stability of the extract is enhanced, 2, 5-dipicolinic acid and L-3-phenyllactic acid are added into the binding system, the hydrogen bonding effect can be preferentially generated with D-configuration xyloside in glycosyl groups contained in the extract, the binding effect is realized by the bridging effect so as to be combined with the pectin, the phenomenon that the binding rate of the extract with D-configuration glycosyl groups and the pectin is low is eliminated, the bioavailability is improved, on the other hand, the hydroxyl and the carboxyl can be combined with amino or amino acid residues of collagen to inhibit the proliferation of collagen cells, the expression level of Connective Tissue Growth Factors (CTGF) of fibers is reduced, the synthesis of the collagen fibers is further reduced, and granulation tissues can not excessively proliferate when skin wounds heal, scar formation is prevented.

The compound emulsion is prepared by the following method: dissolving polyvinyl alcohol to prepare an external water phase with the concentration of 1.5%, adding the external water phase into the micelle according to the weight ratio of 1:6, homogenizing at the rotating speed of 3000rpm for 10min, centrifuging, and precipitating to obtain the water-soluble polyvinyl alcohol. Pigment-containing substances such as anthocyanin in aronia melanocarpa exist stably in a red-yellow-melted salt cation form under an acidic environment, and once the external pH changes, anthocyanin molecules are easy to change in color, so that the color of the soap is influenced negatively, therefore, micelles are wrapped into an emulsion droplet form by using an external water phase, on one hand, the bioactivity of the soap can be protected, the deterioration of the soap can be prevented, on the other hand, the compatibility of the external water phase and a soap base is stronger, the compatibility between an extract and the components of the micelles and the soap base can be increased, and the soap body is prevented from cracking to generate cracks, so that the appearance and the aesthetic degree are influenced.

The soap base for molding is in a molten state; the soap base is melted by heating over water at 50 deg.C. The soap base is melted and then mixed with the multiple emulsion, so that the compatibility of the two substances can be improved, the components in the soap body can be uniformly dispersed, and the evaporation of water in a mixed system can be facilitated, so that the transparency of the soap body is improved, and the appearance is optimized.

The external water phase also contains 3.5 wt% of repellent; the repellent is peppermint oil. The repellent has the effect of repelling mosquitoes, so that the soap has the effect of repelling mosquitoes, is long in repelling time and suitable for various skin conditions, and meanwhile, the components in the repellent can emit the fragrance of natural essential oil, so that the fragrance concentration and the fullness of the soap can be increased, and the addition of industrial essence can be avoided. Preferably, the peppermint oil component stimulates the nerve terminal receptors of the skin, generates a cooling feeling and enriches the sensory experience of the soap.

The aronia melanocarpa soap prepared in the embodiment comprises the following raw materials in parts by weight: 25 parts of aronia melanocarpa extract and 55 parts of soap base. The aronia melanocarpa perfumed soap has the special color and fragrance of aronia melanocarpa fruits, is high in transparency, has the effects of health care and skin care and beauty under the premise of keeping the cleaning effect, and remarkably improves the market competitiveness and the application prospect.

Fig. 1 is a diagram showing the product style of the aronia melanocarpa soap, but the style of the aronia melanocarpa soap manufactured in this embodiment is only used for illustrating the present invention and is not limited to the present invention, and various changes and modifications can be made to the product style of the aronia melanocarpa soap.

Example 2:

the preparation method of the aronia melanocarpa soap comprises the following specific steps:

1) crushing and homogenizing aronia melanocarpa fruits, adding 7 times of double distilled water, extracting at the temperature of 75 ℃ for 1.5h, centrifuging, taking filtrate, and concentrating to obtain an ointment, namely the aronia melanocarpa aqueous extract;

2) taking the centrifugal precipitate obtained in the water extraction step, adding 65% ethanol solution according to the material-liquid ratio of 1:13(g/L), adjusting the pH of the system to 3, sealing the container, placing in an environment at 60 ℃ for 2h, and performing suction filtration on the extract to obtain an organic solvent extract;

3) placing the organic solvent extractive solution in a jar, and adding water vapor at a vapor pressure of 12m³Introducing the liquid with flow rate of/min from the bottom of the tank to escape from the top, continuously introducing for 1.5h, condensing the gas escaping from washing to obtain liquid, performing oil-water separation on the liquid to obtain volatile oil containing a small amount of solvent, heating the oil phase to 80 ℃, preserving heat for 0.5h, removing the organic solvent to obtain aronia melanocarpa volatile oil, and distilling the liquid in the tank under reduced pressure to remove the solvent to obtain an organic solvent extract;

4) respectively taking an aronia melanocarpa aqueous extract, an organic solvent extract and volatile oil according to the proportion of 32 wt%, 36 wt% and 17 wt%, uniformly mixing to form an aronia melanocarpa extract, then adding the extract into a citric acid-sodium hydrogen phosphate buffer solution with the amount of 1.5 times and the pH value of 3.5, uniformly stirring, then adding a pectin solution with the concentration of 50% in an amount of 2.5 times, magnetically stirring, and standing in a dark place at the temperature of 5 ℃ for 10.5 hours to obtain micelles, wherein the buffer solution also contains 0.17 wt% of 2, 5-dipyridyl carboxylic acid and 0.13 wt% of L-3-phenyllactic acid;

5) adding water into polyvinyl alcohol, heating to 70 ℃, stirring until the polyvinyl alcohol is dissolved, preparing an external water phase with the weight concentration of 2.5%, then adding a repellent with the weight ratio of 5%, adding the repellent into micelles with the weight ratio of 1:6, homogenizing at the rotating speed of 3000rpm for 6min, and centrifuging at the speed of 1000r/min for 5min to obtain precipitates, namely, composite emulsion, wherein the repellent contains 55% of peppermint oil and 45% of lemongrass oil;

6) heating the soap to a molten state in a water-proof manner at 55 ℃, adding the compound emulsion while stirring, continuously stirring for 2min, pouring the mixture into a mold for cooling and molding, then demolding, correcting and packaging to obtain the aronia melanocarpa soap, wherein the aronia melanocarpa extract in the soap is 45 parts by weight, and the soap base is 75 parts by weight.

Example 3:

the procedure of this example is substantially the same as that of example 2, and the aronia melanocarpa soap is prepared, except that:

the step 5) comprises the following specific measures: adding water into polyvinyl alcohol, heating to 70 ℃, stirring until the polyvinyl alcohol is dissolved, preparing an external water phase with the weight concentration of 2.5%, then adding a repellent with the weight ratio of 5%, then adding the repellent into a micelle with the weight ratio of 1:6, homogenizing for 6min at the rotating speed of 3000rpm, centrifuging for 5min at the speed of 1000r/min, wherein the obtained precipitate is a multiple emulsion, the external water phase also contains 0.13 wt% of glucurolactone and 0.07 wt% of phosphoglyceride which are cooperated with gelatin and polyvinyl alcohol to form a group with a large space volume by a hydrogen bond hydration system, the group can promote the formation of bubbles, so that the foam fineness of a soap body is improved, meanwhile, a large number of hydrophilic groups can effectively prevent the coagulation of calcium magnesium soap generated in washing, the solubility of the calcium magnesium soap is increased, the viscosity of the calcium magnesium soap is remarkably reduced, the washing capacity of the soap is improved, and the formation of the calcium magnesium soap is prevented by additionally adding a surfactant, the auxiliary material consumption and the production cost are saved.

Example 4:

and 3) not performing steam washing on the organic solvent extracting solution in the step 3), directly performing reduced pressure distillation to remove the solvent to obtain an organic solvent extract, wherein the aronia melanocarpa extract does not contain volatile oil.

Example 5:

step 4) is not carried out, the operation of forming the aronia melanocarpa extract into micelles is directly carried out, and step 5) is directly carried out, so that the aronia melanocarpa extract and the external water phase directly form the multiple emulsion, and the specific operation is as follows: respectively taking the aronia melanocarpa aqueous extract, the organic solvent extract and the volatile oil according to the proportion of 32 wt%, 36 wt% and 17 wt%, uniformly mixing to form the aronia melanocarpa extract, adding water into polyvinyl alcohol, heating to 70 ℃, stirring until the mixture is dissolved, preparing into an external water phase with the weight concentration of 2.5%, then adding a repellent with the weight ratio of 5%, adding the repellent into the extract according to the weight ratio of 1:6, homogenizing for 6min under the condition that the rotating speed is 3000rpm, and centrifuging for 5min at the speed of 1000r/min, wherein the obtained precipitate is the compound emulsion.

Example 6:

2, 5-dipyridyl carboxylic acid and L-3-phenyllactic acid are not added to the citric acid-sodium hydrogen phosphate buffer solution used in the step 4).

Example 7:

the repellent is not added to the external water phase used in the step 5).

Example 8:

the operation of homogenizing the micelles and the external water phase to form the multiple emulsion in the step 5) is not carried out, and the micelles and the repellent formed in the step 4) are directly added into the soap base in a molten state to form the perfumed soap.

Example 9:

and 6) adding an anionic surfactant sodium dodecyl benzene sulfonate with the weight of 4% of the soap base to prepare the perfumed soap.

Test example 1:

antibacterial and mosquito repellent performance test of aronia melanocarpa perfumed soap

(1) And (3) bacteriostatic test: the samples were the soaps prepared in examples 2 and 4, by the following method: by adopting an agar plate culture method, candida albicans, klebsiella pneumoniae, salmonella typhi, pseudomonas aeruginosa, MRSA1 and MRSA2 are used as index bacteria, each bacteria is divided into a test group and a blank control group, and in-vitro bacteriostasis tests are carried out in parallel for 3 times. Preparing a culture medium: taking a proper amount of soap, mashing the soap into powder, accurately weighing 0.3g of soap powder in a 10mL volumetric flask, fixing the volume with high-purity water, and filtering through a filter membrane to remove mixed bacteria to obtain the sterile soap aqueous solution. The prepared sterilized soap aqueous solution was added to a sterilized nutrient agar medium at a volume fraction of 2%, and this was used as a test group. A blank control, i.e. a medium without added aqueous soap solution, was prepared in the same way. Inoculating bacteria: adding 15mL of beef extract culture medium solution into a bacteria bottle, picking 3 similar bacterial colonies into the bacteria bottle by using an aseptic inoculating loop, placing the bacteria bottle in a constant-temperature oscillator for culturing for 4h at 37 ℃, and after the bacterial growth amount reaches a logarithmic growth phase, correcting the bacteria solution to 0.5 McLeod turbidity by using a turbidimeter, namely, OD600 is 0.1; adding 5 mu L of diluted bacterial liquid into each culture medium, uniformly coating the diluted bacterial liquid on the surfaces of the culture medium plates of the test group and the control group, placing the culture medium plates in a constant temperature incubator at about 37 ℃ for 14h, and taking out the culture medium plates. The bacterial reduction amount calculation formula is as follows: bacteria reduction (number of blank colonies-number of test group colonies)/number of blank colonies. The results obtained are shown in table 1 below.

TABLE 1 in vitro bacteriostatic test results of Aronia melanocarpa soap

As can be seen from the above table, the aronia melanocarpa soap has an obvious inhibition effect on the growth of 6 index bacteria which may be contacted with hands, the soap belongs to a broad-spectrum antibacterial soap, and in example 4, part of volatile oil is lost, but the volatile oil contains more fragrant substances, which has a great influence on the fullness of the fragrance concentration of the soap, and has a small influence on the antibacterial activity.

(2) Testing the mosquito repelling effect: the samples were the aronia melanocarpa soaps prepared in examples 2, 4 and 7, and the test method: the method for testing the indoor pesticide effect of the repellent and the evaluation standard are specified in the part of GB/T13917.9-2009 indoor pesticide effect test of the sanitary insecticide for pesticide registration and evaluation of the repellent in part 9 GB/T13917. After the coating, the coating is rinsed for 2 minutes or 15 minutes, and then the effective protection time is respectively tested. Test insects: culex pipiens pallens (Culex pipiens), adult insects which were not bloodborne 4 days after emergence. The test conditions are as follows: the temperature is 26 +/-1 ℃ and the relative humidity is 65 +/-10%, and the data statistics and analysis are shown in the attached figure 2.

Fig. 2 is a schematic diagram of the mosquito repellent effect test result of the aronia melanocarpa soap. As can be seen from the figure, the protection time of flushing after 15min is longer than that of flushing after 2min, and the mosquito repellent effect is the best in example 2, and the effect is the worst in example 7, which indicates that the effect of adding the repellent is better, and the mosquito repellent is more suitable for areas with more mosquitoes or summer; example 2 is superior to example 4, which shows that the volatile oil lost in example 4 contains mosquito repellent components, so the bioavailability of the raw materials in the preparation method of example 2 is better.

Test example 2:

physical properties of aronia melanocarpa soap

(1) Washing and transparency test: the test samples were the soaps prepared in examples 2,5 and 8, and the appearance of the soaps was observed and the soap was washed: the soap is washed on the surface of the soap body by a towel under a tap, all the surfaces are required to be washed, the soap is placed at normal temperature, -5 ℃ and 5 ℃ for 24h respectively after washing, the appearance is observed whether cracks exist after 10 times of washing, the transparency (6.35 +/-0.15 mm thick slices) of the soap is determined according to QB/T2485 plus 2008 soap standard appendix A, and/% > 25. The results are shown in table 2 below.

Table 2 aronia melanocarpa soap quality test

	Before washing	After 10 times of washing
			Example 2	No crack, transparency 29.6	No crack, unchanged color and transparency 29.4
Example 5	No crack, transparency 29.2	No crack, light color, transparency 28.8
			Example 8	No crack, transparency 26.8	Has little crack, light color and transparency of 25.3

As can be seen from the above table, the initial transparency of the toilet soap prepared in example 8 is lower than that of the toilet soaps prepared in examples 2 and 5, after the washing test, the toilet soap prepared in example 2 has no influence, and the transparency of example 5 is slightly reduced but the difference is not significant, but the active ingredients are easily lost due to the protection of the extract by micelle-free, wherein the color-developing substance loss is represented by the lightening of the color of the soap body; example 8 after washing, the transparency is significantly reduced and a small amount of cracks are generated, which indicates that the soap body is unstable, and the existence of the external water phase can increase the compatibility of the soap base and the micelles, prevent the crack generation of the soap body and influence the aesthetic degree of the soap body.

(2) High temperature stability test: the samples were the soaps prepared in examples 2,5 and 6, test method: placing the soap at 55 ℃, storing for 60 days, sampling every 10 days, measuring the content of active ingredients at room temperature, taking the content of anthocyanin as a test standard, taking an anthocyanin solution with the same concentration as a reference, and calculating the retention rate of anthocyanin, wherein the retention rate is taken as a test result of the stability of the aronia melanocarpa extract in the soap at high temperature. The data and analysis are shown in FIG. 3.

Fig. 3 is a schematic diagram showing the stability change of the extract in the aronia melanocarpa soap under a high-temperature storage condition. The soap body of the sample soap has no cracks during storage, but has changed color. The least decrease rate of the retention rate in example 2, the 6 times of example 6, and the most decrease rate in example 5 show that the combination rate of the extract and pectin can be improved more than the preparation method in example 6, so that the stability during high-temperature storage is excellent, and the rapid degradation of the extract at high temperature can be relieved or inhibited more than the preparation method in example 5, so that the color and the health efficacy of the active substances of the soap can be protected, and the shelf life of the soap can be prolonged.

(3) And (3) testing foaming force effect: samples were prepared for toilet soaps prepared in accordance with

preparation methods

2, 3 and 9, and foaming force of the soap was measured by GB/T7462-1994 using 1.5mol/L calcium hard water (5min/mL), and the results are shown in Table 3 below.

Table 3 results of the wash foamability effect test of aronia melanocarpa soap

	Foaming power, min/mL
		Example 2	482
Example 3	495
		Example 9	497

As can be seen from the above table, the foaming ability of example 9 is significantly improved compared to example 2 after the addition of the anionic surfactant, but the difference is not so great as example 3, but the surfactant has greater skin irritation, so the use thereof should be avoided or reduced in actual production; example 3 is higher than example 2 in foaming ability, which shows that the preparation method of example 3 can improve the rich and fine degree of foam of the soap body, effectively prevent the coagulation of calcium-magnesium soap generated in washing, and save the amount of auxiliary materials and production cost.

Test example 3:

test of Aronia melanocarpa perfumed soap for inhibiting scar hyperplasia

The test samples were the soaps prepared in examples 2 and 6, and the test methods were as follows: carrying out epidermal skin wound modeling on a test mouse, wherein the length and the depth of each wound are the same for each male and female half of the test mouse, the soap is used for cleaning the wound 3 times a day for 3min each time, one group without the soap is used as a control group, the test period is 7 days, and the expression of the Connective Tissue Growth Factor (CTGF) antigen in the wound area is detected every day, and the method comprises the following steps: dewaxing and hydrating the tissue of the wound area, incubating for 10min by hydrogen peroxide with the concentration of 3%, blocking endogenous peroxidase, washing by PBS, dropwise adding primary antibody, incubating for 2 hours at 37 ℃, washing, dropwise adding secondary antibody, incubating for 30min at 37 ℃, washing, selecting DBA color developing agent for color development, washing by distilled water, counterstaining, dehydrating and transparentizing, sealing by using a sealing agent, and observing the expression density condition of antigen positive cells under a light microscope, wherein the result is shown in figure 4.

Fig. 4 is a schematic diagram showing the effect of aronia melanocarpa soap on changes in CTGF immunohistochemical density values of wound area tissues. It can be seen from the figure that the density value in example 2 increases most slowly, reaches the highest value on day 3, and begins to decrease rapidly on day four, while the density values in example 6 and the control group are higher than those in example 2, and reach the maximum value only on day four and begin to decrease on day 5 in the two groups, which shows that the perfumed soap in example 2 can significantly inhibit the expression of the fibrous connective tissue growth factor, so that the synthesis of collagen fibers is reduced, granulation tissue does not excessively proliferate when skin wounds heal, and scar formation is prevented, although example 6 also shows a certain inhibition effect on the expression of the fibrous connective tissue growth factor compared with the control group, the effect is not as significant as that of example 2.

Conventional techniques in the above embodiments are known to those skilled in the art, and therefore, will not be described in detail herein.

The above embodiments are merely illustrative, and not restrictive, and those skilled in the art can make various changes and modifications without departing from the spirit and scope of the invention. Therefore, all equivalent technical solutions also belong to the scope of the present invention, and the protection scope of the present invention should be defined by the claims.

Claims

1. The preparation method of the aronia melanocarpa perfumed soap comprises the following steps,

providing an aronia melanocarpa extract;

providing an acidic environment and dispersing the aronia melanocarpa extract in a protective colloid to form micelles;

providing an external water phase, and dispersing the micelles in the external water phase to obtain a multiple emulsion;

providing a soap base, mixing the compound emulsion with the soap base, and molding to obtain the aronia melanocarpa perfumed soap;

the protective colloid is pectin, and a surfactant is not additionally added into the aronia melanocarpa soap;

the Aronia melanocarpa extract comprises 15-35wt% of water extract, 30-45wt% of organic solvent extract and 5-20wt% of Aronia melanocarpa volatile oil;

the micelle is prepared by the following method: dispersing Aronia melanocarpa extract in acidic environment with pH of 2.5-3.5, adding 45-60% pectin solution, magnetically stirring, and standing in dark at 0-5 deg.C for 10-12 hr to obtain micelle;

the acidic environment is provided by a citric acid-sodium hydrogen phosphate buffer solution; the buffer solution also contains 0.1 to 0.5 weight percent of 2, 5-dipyridyl carboxylic acid and 0.05 to 0.2 weight percent of L-3-phenyllactic acid;

the multiple emulsion is prepared by the following method: dissolving polyvinyl alcohol to prepare an external water phase with the concentration of 1-3%, adding the external water phase into a micelle according to the weight ratio of 1:5-8, homogenizing at the rotation speed of 3000-.

2. The method of preparing an aronia melanocarpa soap according to claim 1, wherein: the extraction conditions for preparing the organic solvent extract are as follows: the feed-liquid ratio is 1g:10-20L, the pH is 2-4, the temperature is 50-60 ℃, and the time is 1.5-2.5 h.

3. The method of making an aronia melanocarpa soap as in claim 1, wherein the aronia melanocarpa soap is prepared by a process comprising the steps ofThe method comprises the following steps: the aronia melanocarpa volatile oil is prepared by the following steps: the flow rate is 5-20m³Continuously washing the organic solvent extract with water vapor/min for 1-2 hr, collecting and condensing the gas, separating oil and water, and keeping the temperature of oil phase at 75-90 deg.C for 0.5-1 hr to obtain Aronia melanocarpa volatile oil.

4. The method of preparing an aronia melanocarpa soap according to claim 1, wherein: the extraction steps of the aqueous extract are as follows: crushing and homogenizing the aronia melanocarpa fruits, adding double distilled water of which the amount is 5-8 times of that of the aronia melanocarpa fruits, extracting for 1-2 hours at the temperature of 60-85 ℃, centrifuging, taking filtrate, and concentrating to obtain paste, namely the aronia melanocarpa aqueous extract.

5. The method of preparing an aronia melanocarpa soap according to claim 1, wherein: the soap base for molding is in a molten state; the molten soap base is heated in a water-proof way, and the temperature is 45-55 ℃.

6. The method of preparing an aronia melanocarpa soap according to claim 1, wherein: the external water phase also contains 3-10wt% of repellent; the repellent is at least one of anophelifuge, lemongrass oil, oleum Menthae Dementholatum, and geranium oil.

7. The aronia melanocarpa soap prepared by the preparation method as set forth in any one of claims 1 to 6, wherein: the aronia melanocarpa soap comprises the following raw materials in parts by weight: 4-45 parts of aronia melanocarpa extract and 55-95 parts of soap base.