CN113197829A

CN113197829A - Anti-hair-loss hair-care essence and preparation method thereof

Info

Publication number: CN113197829A
Application number: CN202110474571.9A
Authority: CN
Inventors: 代晓丽; 车小飞
Original assignee: Individual
Current assignee: Shanghai Zhicai Biotechnology Co.,Ltd.
Priority date: 2021-04-29
Filing date: 2021-04-29
Publication date: 2021-08-03
Anticipated expiration: 2041-04-29
Also published as: CN113197829B; CN115252528A; CN115252528B

Abstract

The anti-hair-loss hair care essence is characterized in that: the essence consists of a component A, a component B, a component C, a component D, sorbitan fatty acid ester, sucrose fatty acid ester, Chinese honeylocust fruit extract, seaweed gel and purified water; the composition comprises a component A and a component D, wherein the component A comprises fructus cnidii, semen cuscutae, tea seed meal, fructus kochiae, cordyceps sinensis, gallnut, ginger, American ginseng and an ethanol aqueous solution, the component B comprises a juniper berry extract, thyme essential oil, lavender essential oil, sweet orange oil, peppermint oil, clove oil and an ethanol aqueous solution, the component C comprises beeswax, petrolatum, sucrose wax and an ethanol aqueous solution, and the component D comprises omega-3 fatty acid, vitamin A, vitamin D, folic acid, lysine, an oyster extract and an ethanol aqueous solution. The hair loss preventing and protecting essence prepared by the invention optimizes the head ecological environment, thereby promoting the hair roots to absorb nutrition, thickening the hair, enhancing the toughness, promoting the growth of new hairs and simultaneously inhibiting the original hair in hair follicles from dropping.

Description

Anti-hair-loss hair-care essence and preparation method thereof

Technical Field

The invention relates to the technical field of daily chemical nursing, in particular to an anti-hair loss and hair care essence and a preparation method thereof.

Background

With the increase of social economy and the polarization of working and living environments of people, alopecia, hair withering and yellow, thinning and embrittling cause broken hair, which becomes one of common stubborn diseases, and especially the hair loss is aged. With more attention paid to hair and scalp care, the washing and caring products with real hair loss prevention and hair care effects have great market potential.

Alopecia can be classified into normal alopecia and pathologic alopecia according to the difference of the cause. Normal alopecia is caused by the metabolism of hair follicle cells of the scalp and belongs to the normal metabolism of the human body; pathological alopecia refers to the loss of normal hair follicle cells caused by the lack of nutrition due to degeneration or telogen. Pathological hair loss is caused by a variety of factors: hereditary factors, excessive secretion of male hormones, mental stress, emotional instability, insufficient sleep, overeating high-fat foods, chronic poisoning, deficiency of trace elements, low stress capability, autoimmune endocrine function disorder, menstrual disorder and postpartum dysregulation, etc. These factors cause deterioration of head ecological environment such as unbalance of scalp nutrition supply, poor blood circulation, excessive fat, hair follicle obstruction, etc., thereby preventing nutrient absorption by hair roots, affecting hair growth, and causing alopecia. In addition, hair loss can also be caused or accelerated by external factors such as hair coloring, hair waving, hair drying, intense sun exposure, radiation, environmental and chemical shampoo pollution, and excessive or insufficient air humidity. Alopecia is characterized by fine hair diameter, reduced hair density, and alopecia, and till alopecia of different degrees appears, and is usually accompanied by symptoms such as increased scalp oil secretion.

At present, in the hair loss prevention and care products in the market, a large amount of chemicals such as synthetic surfactants, synthetic hormones for promoting hair growth and the like are used, so that skin is stimulated in the process of nursing, scalp injury is caused, and obvious side effects can be caused after long-term use. Some nursing products adopt natural raw materials to prepare anti-hair loss and hair care products, but the nursing effect cannot be achieved, the main reason is that natural extracts (essential oil) are high in volatility and are volatilized before being absorbed by the scalp, the scalp difficultly absorbs the components of the natural essential oil, and the effective components cannot permeate into hair follicles of the scalp to play a role. Therefore, the key to solve the above technical problems is to delay the volatilization of the natural essential oil components and promote the effective absorption of the natural essential oil components by the scalp.

Disclosure of Invention

The invention aims to provide a hair loss preventing and protecting essence.

The invention also aims to provide the preparation method of the anti-hair loss and care essence, and the effective components in the juniper berry extract in the prepared anti-hair loss and care essence are not easy to volatilize and can be effectively absorbed and utilized by skin.

The purpose of the invention is realized by the following technical scheme:

the anti-hair-loss hair care essence is characterized in that: the essence comprises, by weight, 50 parts of a component A, 15-20 parts of a component B, 5-10 parts of a component C, 2.5-5 parts of a component D, 0.5-1.5 parts of sorbitan fatty acid ester, 1-1.5 parts of sucrose fatty acid ester, 0.5-1 part of a saponin extract and 0.5-2 parts of seaweed gel, and the balance of purified water is 100 parts, wherein the component A and the component B are mixed, the sorbitan fatty acid ester, the sucrose fatty acid ester and the saponin extract are added and stirred at a high speed to form a micro emulsion, the component D and the seaweed gel are added into the micro emulsion and stirred at a low speed, then the component C is added, and the purified water is added to 100 parts and stirred continuously; the component A is prepared by adding 1-2 parts of fructus cnidii, 2-3 parts of semen cuscutae, 1-3 parts of tea seed meal, 1-2 parts of fructus kochiae, 0.01-0.08 part of cordyceps sinensis, 1-3 parts of gallnut, 2-3 parts of ginger and 0.2-0.8 part of American ginseng into 40-50 parts of ethanol water solution with volume concentration of 50% for reflux extraction, the component B is prepared by 4-7 parts of juniper berry extract, 0.5-1 part of thyme essential oil, 1-2 parts of lavender essential oil, 0.5-1.2 parts of sweet orange oil, 1-1.5 parts of peppermint oil, 0.1-0.5 part of clove oil and 20 parts of ethanol water solution with volume concentration of 50%, the component C is prepared by 2-3 parts of beeswax, 1-3 parts of petrolatum, 1-2 parts of cane wax and 20 parts of ethanol water solution with volume concentration of 50%, and the component D is prepared by 0.5-2 parts of omega-3 fatty acid, 0.5-0.8 parts of vitamin A and 0.8-0.8 part of vitamin D, 0.4-1 part of folic acid, 0.5-1 part of lysine, 0.1-0.6 part of oyster extract and 10 parts of 50% ethanol aqueous solution.

The cone of juniper berries (i.e., juniper berries) turns from green to black or dark blue after ripening, which is the main site for extracting juniper berry essential oil. Although juniper berries or branches and leaves can also extract essential oil, which is called juniper essential oil, the juniper berries or branches and leaves have poor effective components, low value and certain hair care effect, but the juniper berries essential oil rather than the juniper berries essential oil is selected to be used for preventing alopecia due to poor alopecia preventing effect.

The hair conditioner adopts pure natural components, such as fructus cnidii, semen cuscutae, tea seed meal, fructus kochiae, cordyceps sinensis, gallnut, ginger and American ginseng, and the components have the effects of nourishing and protecting hair and scalp. The invention also adds various essential oils, such as thyme essential oil, lavender essential oil, sweet orange oil, peppermint oil and clove oil, and the juniper berry extract (juniper berry essential oil) effectively plays the role in the system: providing nutrients and trace elements for hair growth; dredging pores, promoting blood circulation, sterilizing, improving hair production environment, and promoting scalp and hair health, thereby preventing alopecia, broken hair, and scalp breeding.

However, the juniper berry essential oil is easier to volatilize than the juniper berry essential oil, and when the juniper berry essential oil is used for preparing an anti-hair loss hair care product, the juniper berry essential oil can volatilize quickly after being absorbed by the scalp, so that the anti-hair loss hair care effect of the juniper berry essential oil cannot be effectively exerted; in addition, the juniper berry essential oil mainly contains various effective components such as borneol, terpineol, terpinene, cadinene, cedrene, camphene and the like, most of the effective components are difficult to be completely absorbed by the scalp on the surface layer of the scalp, so that the hair loss preventing and protecting effect is not obvious, the hair protecting components adopted in the essence are various, the effective components in the juniper berry essential oil are more, the prepared hair loss preventing and protecting essence is easy to be layered and settled, the scalp cannot effectively absorb the functional components, and a large number of scalp problems are increased.

The active ingredients in the juniper berry extract (juniper berry essential oil) comprise borneol, terpineol, terpinene, cadinene, cedrene, camphene and the like, and the active ingredients are found to have quite high compatibility with omega-3 fatty acid and vitamin A in the D component in the preparation process, and the omega-3 fatty acid and the vitamin A play a role of a carrier in the scalp absorption process, so that the active ingredients in the juniper berry extract rapidly enter hair follicles through the omega-3 fatty acid and the vitamin A and are absorbed by the scalp together. The seaweed gel is promoted to form a gel with higher viscosity, and the active ingredients in the juniper berry essential oil are effectively and uniformly dispersed in the gel while the vitamin as a carrier participates in the formation of the gel through high compatibility with the vitamin while the gel is formed, so that an effective stable system structure is formed, and the sedimentation and layering of the active ingredients in the juniper berry essential oil are prevented.

The beeswax in the component C is used as a suspending agent in the microemulsion to improve the stability of a microemulsion system, secondly, the beeswax, petrolatum, sucrose wax and seaweed gel in the component C are bonded on the surface of a colloidal structure to form a complete, staggered and compact blending semipermeable membrane, the semipermeable membrane on the surface of the colloid forms physical barrier to active ingredients in the juniper berry extract to inhibit volatilization of the active ingredients, secondly, the oyster extract in the component D contains a large amount of ions such as inorganic salt, calcium, iron, selenium and zinc to provide abundant trace elements for scalp and promote growth of scalp and hair, and the ions are also complexed with groups such as hydroxyl, olefin and the like rich in the juniper berry essential oil to form chemical inhibition and are effectively wrapped in gel colloid to be uniformly dispersed along with omega-3 fatty acid and vitamin carriers, so that the volatilization of the active ingredients in the juniper berry essential oil is inhibited.

The preparation method of the anti-hair-loss and hair-care essence is characterized by comprising the following steps: firstly, preparing a juniper berry extract, mixing common cnidium fruit, south dodder seed, tea seed meal, belvedere fruit, cordyceps sinensis, Chinese gall, ginger and American ginseng, adding an ethanol aqueous solution, heating, refluxing and extracting, adding medicinal-grade active carbon, stirring and filtering to form a component A, adding thyme essential oil, lavender essential oil, sweet orange oil, peppermint oil, clove oil and juniper berry extract into the ethanol aqueous solution, stirring and mixing uniformly to form a component B, adding beeswax, petrolatum and cane sugar wax into the ethanol aqueous solution, heating and stirring to form a component C, adding omega-3 fatty acid, vitamin A, vitamin D, folic acid, lysine and oyster extract into the ethanol aqueous solution, and stirring at normal temperature to form a component D; mixing the component A and the component B, adding sorbitan fatty acid ester, sucrose fatty acid ester and saponin extract, stirring at a high speed to form a micro emulsion, simultaneously adding the component D and seaweed gel into the micro emulsion under low-speed stirring, then adding the component C, adding purified water to make up 100 parts, and continuously stirring for 30-50 min.

Further, the high-speed stirring is carried out at 1200-1500 rpm for 20-30 min, and the low-speed stirring is carried out at 20-30 rpm for 50-70 min.

Further, the preparation of the juniper berry extract is specifically that mature juniper berries are cleaned and dried, a mixture consisting of absolute ethyl alcohol and isopropyl ether according to a mass ratio of 1: 2-5 is added to form a mixed solution 1, the mixed solution is heated and extracted in a nitrogen atmosphere, and then the mixed solution is filtered to obtain an extract solution 1; adding purified water and ethanol into the same juniper berries according to a ratio of 1: 1-2 to form a mixture 2, heating, performing reflux extraction, filtering to obtain an extract 2, mixing the extract 1 and the extract 2 to form a mixed extract, performing reduced pressure distillation, collecting a fraction 1, a fraction 2, a fraction 3 and a fraction 4 in sections, and mixing to form a juniper berry extract, namely, juniper berry essential oil.

In the process of preparing the juniper berry essential oil, the extraction liquid 1 and the extraction liquid 2 are respectively prepared, and an oily compound and an aqueous compound are effectively extracted, so that the effective components in the essential oil are diversified and contain more high-purity anti-hair loss and hair care functional components, pressure change is controlled in the process of reduced pressure evaporation, fractions are collected in sections by adjusting distillation temperature and are mixed in proportion to form the juniper berry essential oil with optimal balance of volatilization speed and absorption effect, the volatilization speed of the prepared juniper berry essential oil is reduced, the capability of the prepared juniper berry essential oil effectively absorbed by scalp is improved, and the problem that the prepared juniper berry essential oil is difficult to absorb by scalp due to the improvement of the distillation temperature is solved. The juniper berry essential oil composed of different fractions contains more abundant functional groups, improves the compatibility of the juniper berry essential oil in omega-3 fatty acid and vitamin, and the complexing ability of the juniper berry essential oil and ions in the oyster extract, thereby enhancing the anti-volatility and scalp absorption ability of the juniper berry essential oil.

Furthermore, the mass ratio of the juniper berries to the mixture in the mixed liquid 1 is 2-3: 10-12, and the mass ratio of the juniper berries to the mixture in the mixed liquid 2 is 1-3: 8-10.

Further, the preparation of the extraction liquid 1 is specifically to heat the mixed liquid 1 to 60-75 ℃, introduce nitrogen gas, maintain the pressure at 1.0-1.2 MPa, extract for 3-4 h, then cool to 5-10 ℃, release the pressure, filter and separate to obtain the extraction liquid 1.

Further, the preparation of the extraction liquid 2 is specifically to heat the mixed liquid 2 to 100-110 ℃ for reflux extraction for 5-6 h, then cool the mixed liquid to 20-30 ℃, filter and separate to obtain the extraction liquid 2.

Further, the extract liquor 1 and the extract liquor 2 form mixed extract liquor according to the mass ratio of 1: 1.6-2.

Further, the step of collecting fractions in a segmented mode is to conduct reduced pressure distillation on the mixed extraction liquid at the temperature of 30-40 ℃ and under the absolute pressure of 500-1000 Pa, then reduce the absolute pressure to 50Pa, and collect fraction 1.

Further, maintaining the absolute pressure at 30-50 Pa, heating to 60-100 deg.C at a rate of 0.5-1 deg.C/min to collect fraction 2, continuously heating to 110-150 deg.C to collect fraction 3, and heating to 160-180 deg.C to collect fraction 4.

Further, the fraction 1, the fraction 2, the fraction 3 and the fraction 4 are mixed in a mass ratio of 0.1-0.5: 0.2-0.5: 0.5-1: 0.3-0.5 to form the juniper berry extract.

Most specifically, the preparation method of the anti-hair-loss and hair-care essence is characterized by comprising the following steps of:

step 1, preparation of juniper berry extract

(1) Cleaning and drying mature juniper berries, adding a mixture consisting of absolute ethyl alcohol and isopropyl ether according to a mass ratio of 1: 2-5 to form a mixed solution 1, heating to 60-75 ℃ in a nitrogen atmosphere with the pressure of 1.0-1.2 MPa, extracting for 3-4 h, then cooling to 5-10 ℃, decompressing, filtering and separating to obtain an extract 1; adding the same juniper berries into a mixture composed of purified water and ethanol in a ratio of 1: 1-2 to form a mixed solution 2, heating to 100-110 ℃, performing reflux extraction for 5-6 hours, then cooling to 20-30 ℃, filtering, and separating to obtain an extract solution 2, wherein the mass ratio of the juniper berries to the mixture in the mixed solution 1 is 2-3: 10-12, and the mass ratio of the juniper berries to the mixture in the mixed solution 2 is 1-3: 8-10;

(2) mixing the extract 1 and the extract 2 according to a mass ratio of 1: 1.6-2 to form a mixed extract, distilling for 1h at 30-40 ℃ and an absolute pressure of 500-1000 Pa, keeping the temperature unchanged, reducing the absolute pressure to 50Pa, collecting the fraction 1, heating to 60-100 ℃ at a speed of 0.5-1/° C min, collecting the fraction 2, continuously heating to 110-150 ℃, collecting the fraction 3, continuously heating to 160-180 ℃ and collecting the fraction 4, and mixing the fraction 1, the fraction 2, the fraction 3 and the fraction 4 according to a mass ratio of 0.1-0.5: 0.2-0.5: 0.5-1: 0.3-0.5;

step 2, preparing essence

(1) Form the components

And (2) component A: mixing 1-2 parts by weight of fructus cnidii, 2-3 parts by weight of semen cuscutae, 1-3 parts by weight of tea seed meal, 1-2 parts by weight of fructus kochiae, 0.01-0.08 part by weight of cordyceps sinensis, 1-3 parts by weight of gallnut, 2-3 parts by weight of ginger and 0.2-0.8 part by weight of American ginseng, drying at 40-45 ℃, then crushing to 0.1-0.5 mm, adding 40-50 parts by weight of ethanol water solution, heating for reflux extraction for 4-6 hours, then cooling to 20-30 ℃, and filtering to remove solid matters; adding medical-grade activated carbon, stirring for 1-2 h, and filtering to obtain a transparent liquid;

and (B) component: mixing 0.5-1 part by weight of thyme essential oil, 1-2 parts by weight of lavender essential oil, 0.5-1.2 parts by weight of sweet orange oil, 1-1.5 parts by weight of peppermint oil, 0.1-0.5 part by weight of clove oil and 4-7 parts by weight of juniper berry extract, adding the mixture into 20 parts by weight of ethanol water solution, stirring and mixing;

and (3) component C: adding 2-3 parts by weight of beeswax, 1-3 parts by weight of petrolatum and 1-2 parts by weight of sucrose wax into 20 parts by weight of ethanol water solution, heating to 40-50 ℃, stirring to form transparent solution, and cooling to normal temperature;

and (3) component D: adding 0.5-2 parts of omega-3 fatty acid, 0.1-0.5 part of vitamin A, 0.4-0.8 part of vitamin D, 0.4-1 part of folic acid, 0.5-1 part of lysine and 0.1-0.6 part of oyster extract into 10 parts of ethanol aqueous solution by weight, and stirring at normal temperature to form a transparent solution;

(2) mixing the components

Mixing 50 parts of the component A and 15-20 parts of the component B, adding 0.5-1.5 parts of sorbitan fatty acid ester, 1-1.5 parts of sucrose fatty acid ester and 0.5-1 part of saponin extract, stirring at 1200-1500 rpm for 20-30 min to form a micro-emulsion, adding 2.5-5 parts of the component D and 0.5-2 parts of seaweed gel into the micro-emulsion, stirring at 30-50 rpm for 50-70 min, then adding 5-10 parts of the component C, adding purified water to make up 100 parts, and continuously stirring for 30-50 min.

According to the invention, the preparation links of the juniper berry extract are adopted to regulate and control extraction and reduced pressure distillation, fractions are collected in sections, and the juniper berry extract is prepared by mixing according to a proportion, so that the volatility of the juniper berry extract is reduced, the effective absorption capacity of the juniper berry extract by skin is improved, the juniper berry extract is combined with the process of synthesizing essence to prepare microemulsion, the prepared juniper berry extract is rich in a large amount of functional groups, and is complexed with ions in oyster extract and forms a combined action of blending semipermeable membrane, the volatility of the juniper berry extract is reduced, and the compatibility of the prepared juniper berry extract with omega-3 fatty acid and vitamins is realized, and the omega-3 fatty acid and the vitamins are used as carriers to effectively enter scalp and are quickly absorbed and utilized by scalp, so that the hair loss prevention and care effects of the juniper berry extract are improved. According to the invention, the O/W type microemulsion structure is formed, so that the effective components are solubilized, ions such as calcium and zinc in the oyster extract and seaweed gel are subjected to ion exchange in the presence of vitamins to form a high-viscosity gel structure, the system component structure is stabilized, and the problems of layering, sedimentation and the like of the components in the microemulsion are further prevented.

The invention has the following technical effects:

the juniper berry extract which is an effective component with excellent hair loss prevention function and is contained in the hair loss prevention and care essence prepared by the invention is not easy to mix hair, has strong permeability and can be effectively absorbed by scalp, thereby exerting the excellent hair loss prevention and care effects.

The anti-hair-loss hair-care essence prepared by the invention contains a large amount of functional components beneficial to conditioning scalp and caring hair, ensures balanced nutrition supply of scalp, promotes smooth blood circulation, reduces grease secretion of hair follicles of scalp, dredges hair follicles, optimizes the ecological environment of the head, promotes hair follicles to grow new hair, promotes the hair roots to absorb nutrition, thickens the hair, enhances the toughness, has smooth luster and inhibits the original hair in the hair follicles from falling off. The hair density is increased by 51.9% compared with the hair before use, the hair diameter is increased by 51.1% compared with the hair before use, and the hair loss number is reduced by 57.5% compared with the hair before use.

Detailed Description

The present invention is described in detail below by way of examples, it should be noted that the following examples are only for illustrating the present invention and should not be construed as limiting the scope of the present invention, and those skilled in the art can make some insubstantial modifications and adaptations of the present invention based on the above-mentioned disclosure.

Example 1

A preparation method of the hair loss preventing and protecting essence comprises the following steps:

step 1, preparation of juniper berry extract

(1) Cleaning mature juniper berries, drying at 55 ℃, adding a mixture consisting of absolute ethyl alcohol and isopropyl ether according to a mass ratio of 1:3 to form a mixed solution 1, heating to 70 ℃ under a nitrogen atmosphere with the pressure of 1.1MPa, extracting for 3.5 hours, then cooling to 8 ℃, decompressing, filtering and separating to obtain an extract 1 which is mainly an oil-soluble compound; adding purified water and ethanol into the same juniper berries to form a mixture 2 consisting of 1:1.5, heating to 105 ℃, performing reflux extraction for 5.5 hours, then cooling to 25 ℃, filtering, and separating to obtain an extract 2, wherein the main component of the extract is a water-soluble compound, the mass ratio of the juniper berries to the mixture in the mixture 1 is 2:11, and the mass ratio of the juniper berries to the mixture in the mixture 2 is 2: 9;

(2) mixing the extract 1 and the extract 2 according to a mass ratio of 1:1.8 to form a mixed extract, distilling at 35 ℃ and an absolute pressure of 800Pa for 1h, keeping the temperature unchanged, reducing the absolute pressure to 50Pa, collecting the fraction 1, then heating to 80 ℃ at a speed of 0.8/DEG C min, collecting the fraction 2, continuously heating to 130 ℃, collecting the fraction 3, continuously heating to 170 ℃ and collecting the fraction 4, and mixing the fraction 1, the fraction 2, the fraction 3 and the fraction 4 according to a mass ratio of 0.3:0.4:0.7: 0.4;

step 2, preparing essence

(1) Form the components

And (2) component A: mixing 1.5 parts by weight of fructus cnidii, 2.5 parts by weight of semen cuscutae, 2 parts by weight of tea seed meal, 1.5 parts by weight of fructus kochiae, 0.05 part by weight of cordyceps sinensis, 2 parts by weight of gallnut, 2.5 parts by weight of ginger and 0.6 part by weight of American ginseng, drying at 42 ℃, then crushing to 0.2mm, adding 45 parts by weight of ethanol aqueous solution, heating for reflux extraction for 5 hours, then cooling to 25 ℃, and filtering to remove solid matters; adding medical grade active carbon, stirring for 1.5h, and filtering to obtain transparent liquid;

and (B) component: mixing 0.8 part of thyme essential oil, 1.5 parts of lavender essential oil, 1 part of sweet orange oil, 1.2 parts of peppermint oil, 0.3 part of clove oil and 6 parts of juniper berry extract according to parts by weight, adding into 20 parts of ethanol water solution, stirring and mixing;

and (3) component C: adding 2.5 parts by weight of beeswax, 2 parts by weight of petrolatum and 1.5 parts by weight of sucrose wax into 20 parts by weight of ethanol aqueous solution, heating to 45 ℃, stirring to form transparent solution, and then cooling to normal temperature;

and (3) component D: adding 1 part of omega-3 fatty acid, 0.3 part of vitamin A, 0.6 part of vitamin D, 0.8 part of folic acid, 0.6 part of lysine and 0.5 part of oyster extract into 10 parts of ethanol aqueous solution according to parts by weight, and stirring at normal temperature to form transparent solution;

(2) mixing the components

Mixing 50 parts of component A and 18 parts of component B, adding 1 part of sorbitan fatty acid ester, 1.2 parts of sucrose fatty acid ester and 0.8 part of Chinese honeylocust fruit extract, stirring at 1300rpm for 25min to form a microemulsion, adding 4 parts of component D and 1.5 parts of seaweed gel simultaneously to the microemulsion and stirring at 40rpm for 60min, then adding 6 parts of component C, adding purified water to make up 100 parts, and continuously stirring for 40 min.

Comparative example 1

The preparation method of the anti-hair loss and hair care essence containing the juniper berry extract comprises the following steps:

step 1; preparation of juniper berry extract

(1) Cleaning mature juniper berries, drying at 55 ℃, adding a mixture consisting of absolute ethyl alcohol and isopropyl ether according to a mass ratio of 1:3 to form a mixed solution 1, heating to 70 ℃ under a nitrogen atmosphere with the pressure of 1.1MPa, extracting for 3.5 hours, then cooling to 8 ℃, decompressing, filtering and separating to obtain an extract liquor, wherein the mass ratio of the juniper berries to the mixture in the mixed solution is 2: 11; (2) distilling the extract liquid at 35 ℃ and under the absolute pressure of 800Pa for 1h, keeping the temperature unchanged, reducing the absolute pressure to 50Pa, collecting fraction 1, then heating to 130 ℃, collecting fraction 2, and mixing fraction 1 and fraction 2 according to the mass ratio of 3: 7;

step 2: preparation of essence

(1) Form the components

Component A, component C and component D, which were the same as in example 1, were mixed in the same manner as in example 1, except that the extract of juniper berries prepared in comparative example 2 was used in place of the extract of juniper berries prepared in example 1 to prepare component B.

Comparative example 2

step 1; preparation of juniper berry extract

The juniper berry extract was prepared in the same manner as in example 1.

Step 2: preparation of essence

(1) Form the components

The same components A and B as in example 1 were used; and (3) component C: adding 2.5 parts by weight of beeswax into 15 parts by weight of ethanol water solution, heating to 45 ℃, stirring, and then cooling to normal temperature; and (3) component D: adding 0.8 part of vitamin D, 0.8 part of folic acid and 0.6 part of lysine into 10 parts of ethanol aqueous solution according to parts by weight, and stirring at normal temperature to form transparent solution;

(2) mixing the components

Mixing 50 parts of component A and 18 parts of component B, adding 1 part of sorbitan fatty acid ester, 1.2 parts of sucrose fatty acid ester and 0.8 part of Chinese honeylocust fruit extract, stirring at 1400rpm for 25min to form a micro emulsion, sequentially adding 2 parts of component C, 4 parts of component D and seaweed gel, stirring at 40rpm for 60min, supplementing water until the total weight is 100 parts, and continuously stirring for 40 min.

Example 2

step 1, preparation of juniper berry extract

(1) Cleaning mature juniper berries, drying at 60 ℃, adding a mixture consisting of absolute ethyl alcohol and isopropyl ether according to a mass ratio of 1:2 to form a mixed solution 1, heating to 60 ℃ in a nitrogen atmosphere with the pressure of 1.0MPa, extracting for 4 hours, then cooling to 5 ℃, decompressing, filtering and separating to obtain an extract 1; adding purified water and ethanol into the same juniper berries to form a mixture 2 according to a ratio of 1:1, heating to 100 ℃, performing reflux extraction for 6 hours, then cooling to 20 ℃, filtering, and separating to obtain an extract 2, wherein the mass ratio of the juniper berries to the mixture in the mixture 1 is 2:10, and the mass ratio of the juniper berries to the mixture in the mixture 2 is 1: 8;

(2) mixing the extract 1 and the extract 2 according to a mass ratio of 1:1.6 to form a mixed extract, distilling at 30 ℃ and an absolute pressure of 500Pa for 1h, keeping the temperature unchanged, reducing the absolute pressure to 50Pa, collecting the fraction 1, then heating to 60 ℃ at a speed of 0.5/DEG C min, collecting the fraction 2, continuously heating to 110 ℃, collecting the fraction 3, continuously heating to 160 ℃ and collecting the fraction 4, and mixing the fraction 1, the fraction 2, the fraction 3 and the fraction 4 according to a mass ratio of 0.1:0.2:0.5: 0.5;

step 2, preparing essence

(1) Form the components

And (2) component A: mixing 1 part of fructus cnidii, 2 parts of semen cuscutae, 1 part of tea seed meal, 1 part of fructus kochiae, 0.08 part of cordyceps sinensis, 1 part of gallnut, 3 parts of ginger and 0.8 part of American ginseng according to parts by weight, drying at 40 ℃, then crushing to 0.1mm, adding 40 parts of ethanol aqueous solution, heating, carrying out reflux extraction for 6 hours, then cooling to 20 ℃, and filtering to remove solid matters; adding medical grade active carbon, stirring for 1h, and filtering to obtain transparent liquid;

and (B) component: mixing 0.5 part of thyme essential oil, 2 parts of lavender essential oil, 0.5 part of sweet orange oil, 1.5 parts of peppermint oil, 0.1 part of clove oil and 4 parts of juniper berry extract according to parts by weight, adding into 20 parts of ethanol water solution, and stirring and mixing;

and (3) component C: adding 2 parts by weight of beeswax, 3 parts by weight of petrolatum and 1 part by weight of sucrose wax into 20 parts by weight of ethanol aqueous solution, heating to 40 ℃, stirring to form transparent solution, and then cooling to normal temperature;

and (3) component D: adding 0.5 part of omega-3 fatty acid, 0.5 part of vitamin A, 0.4 part of vitamin D, 1 part of folic acid, 0.5 part of lysine and 0.1 part of oyster extract into 10 parts of ethanol aqueous solution by weight, and stirring at normal temperature to form transparent solution;

(2) mixing the components

Mixing 50 parts of component A and 15 parts of component B, adding 0.5 part of sorbitan fatty acid ester, 1 part of sucrose fatty acid ester and 0.5 part of Chinese honey locust extract, stirring at 1200rpm for 30min to form a microemulsion, adding 2.5 parts of component D and 0.5 part of alginate jelly to the microemulsion and stirring at 30rpm for 70min, then adding 5 parts of component C, adding purified water to make up 100 parts, and continuously stirring for 30 min.

Example 3

step 1, preparation of juniper berry extract

(1) Cleaning mature juniper berries, drying at 50 ℃, adding a mixture consisting of absolute ethyl alcohol and isopropyl ether according to a mass ratio of 1:5 to form a mixed solution 1, heating to 75 ℃ in a nitrogen atmosphere with the pressure of 1.2MPa, extracting for 3 hours, then cooling to 10 ℃, decompressing, filtering and separating to obtain an extract 1; adding purified water and ethanol into the same juniper berries to form a mixture 2 according to a ratio of 1:2, heating to 110 ℃, performing reflux extraction for 5 hours, then cooling to 30 ℃, filtering, and separating to obtain an extract 2, wherein the mass ratio of the juniper berries to the mixture in the mixture 1 is 3:12, and the mass ratio of the juniper berries to the mixture in the mixture 2 is 3: 10;

(2) mixing the extract 1 and the extract 2 according to a mass ratio of 1:2 to form a mixed extract, distilling at 40 ℃ and an absolute pressure of 1000Pa for 1h, keeping the temperature unchanged, reducing the absolute pressure to 50Pa, collecting the fraction 1, then heating to 100 ℃ at a speed of 1/DEG C min, collecting the fraction 2, continuously heating to 150 ℃, collecting the fraction 3, continuously heating to 180 ℃ and collecting the fraction 4, and mixing the fraction 1, the fraction 2, the fraction 3 and the fraction 4 according to a mass ratio of 0.5:0.5:1: 0.3;

step 2, preparing essence

(1) Form the components

And (2) component A: mixing 2 parts by weight of fructus cnidii, 3 parts by weight of semen cuscutae, 3 parts by weight of tea seed meal, 2 parts by weight of fructus kochiae, 0.01 part by weight of cordyceps sinensis, 3 parts by weight of gallnut, 2 parts by weight of ginger and 0.2 part by weight of American ginseng, drying at 45 ℃, then crushing to 0.5mm, adding 50 parts by weight of ethanol aqueous solution, heating, performing reflux extraction for 6 hours, then cooling to 20 ℃, and filtering to remove solid matters; adding medical grade active carbon, stirring for 2h, and filtering to obtain transparent liquid;

and (B) component: mixing 1 part by weight of thyme essential oil, 1 part by weight of lavender essential oil, 1.2 parts by weight of sweet orange oil, 1 part by weight of peppermint oil, 0.5 part by weight of clove oil and 7 parts by weight of juniper berry extract, adding into 20 parts by weight of ethanol water solution, stirring and mixing;

and (3) component C: adding 3 parts by weight of beeswax, 1 part by weight of petrolatum and 2 parts by weight of sucrose wax into 20 parts by weight of ethanol aqueous solution, heating to 50 ℃, stirring to form transparent solution, and then cooling to normal temperature;

and (3) component D: adding 2 parts by weight of omega-3 fatty acid, 0.1 part by weight of vitamin A, 0.8 part by weight of vitamin D, 0.4 part by weight of folic acid, 1 part by weight of lysine and 0.6 part by weight of oyster extract into 10 parts by weight of ethanol aqueous solution, and stirring at normal temperature to form transparent solution;

(2) mixing the components

Mixing 50 parts of component A and 20 parts of component B, adding 1.5 parts of sorbitan fatty acid ester, 1.5 parts of sucrose fatty acid ester and 1 part of Chinese honeylocust fruit extract, stirring at 1500rpm for 20min to form a microemulsion, adding 5 parts of component D and 2 parts of seaweed gel to the microemulsion, stirring at 50rpm for 50min, then adding 5 parts of component C, adding purified water to make up 100 parts, and continuously stirring for 50 min.

The hair loss preventing and caring essence prepared by the invention and the hair loss preventing and caring essence prepared by the comparative examples 1 and 2 are subjected to relevant detection and comparison.

1. Volatility test

Two pieces of glass with the same area are taken, cleaned and wiped dry, then equal amounts of the juniper berry extract prepared in example 1 and the juniper berry extract prepared in comparative example 1 are respectively smeared on the surface of the glass, the glass is placed for 30min under the same environment (the temperature and the humidity are the same), then equal amounts of ethanol are used for cleaning the glass (the cleaning is ensured), and then the concentration of the juniper berry extract in the ethanol is measured. Calculating the residual quantity of the essence according to the concentration, and finally calculating the volatility kappa: κ ═ (m1-m2)/m1 × 100%, m1 is the mass of the original smear; m2 is the mass after volatilization.

The same test method is adopted to test the volatility of the effective components of the juniper berry extract in the anti-hair loss and hair care essence prepared by the invention and the anti-hair loss and hair care essence prepared by the comparative example 1 and the comparative example 2, and the experiment is repeated for a plurality of times, and the experimental results are shown in the table 1.

Table 1: juniper berry extracts prepared according to the invention and comparative examples and their volatility in hair care lotions.

As can be seen from the above, the juniper berry extract prepared in comparative example 1 has a large volatility, the hair care essence prepared in comparative example 1 has a remarkably suppressed control of the volatility of essential oils, comparative example 2 has less sucrose wax, omega-3 fatty acids, vitamin a and oyster shell extract than in example 1, and the addition order is different from example 1, and the juniper berry extract in the anti-hair loss hair care essence prepared in comparative example 2 has a significantly lower volatility than that of the present invention. According to the invention, sucrose wax, petrolatum, beeswax and seaweed gel are bonded on the surface of the colloidal structure to form a staggered and compact blending semipermeable membrane for inhibiting volatilization of active ingredients, the oyster extract and the juniper berries are extracted to form complexation for retaining volatile ingredients, and vitamins and seaweed gel in the microemulsion form gel, so that the volatility of the juniper berries extract is further reduced, the active ingredients of the juniper berries extract are well retained, and favorable conditions are provided for scalp absorption of the active ingredients. The juniper berry extract prepared by the invention has lower volatility, and Ca in the oyster extract is added in the process of preparing essence²⁺、Zn²⁺With Na in seaweed gel⁺Ion exchange is formed, a colloidal structure with higher viscosity is formed with vitamin A, D, beeswax, petrolatum, sucrose wax and seaweed gel are combined, a staggered and compact blending semipermeable membrane is formed on the surface of the colloidal structure to form physical barrier, the oyster extract contains inorganic salt, calcium, iron, zinc and other ions, and the ions are complexed with groups such as hydroxyl, olefin and the like rich in the juniper berry essential oil to form chemical inhibition, so that volatilization of active ingredients in the juniper berry essential oil is inhibited.

2. In vitro transdermal test (Permeability test)

Taking a healthy SPF male mouse, weighing (20 +/-2) g, removing the neck of the male mouse, killing the male mouse, taking the abdominal skin of the male mouse, removing a fat layer, scraping the mouse hair on the skin of the male mouse, washing the male mouse with physiological saline, fixing the skin of the male mouse between a diffusion pool and a receiving pool, wherein the cuticle layer of the skin faces the diffusion pool, the dermis layer faces the receiving pool and is just contacted with a solvent in the receiving pool to prevent bubbles from being generated. The volume of the receiving cell was 15 mL. Placing the essence lmL in a diffusion cell, adding distilled water into a receiving cell with a magnetic stirrer, placing the receiving cell on a magnetic stirrer of an intelligent transdermal tester, setting the water bath temperature at 37 ℃, stirring at the speed of 350r/min, sampling every 5min, and sampling through a sampling port (simultaneously supplementing an equal amount of receiving liquid) for analysis.

Table 2: permeability of the hair loss preventing and caring essence prepared in the present invention and comparative example 1.

The permeation rate of the hair care essence prepared by the invention is higher than that of the hair care essences prepared by the comparative examples 1 and 2 in the same permeation time, and the detection shows that the content of the active ingredients of the juniper berry extract in the rest of the anti-hair-loss hair care essences in the diffusion cells corresponding to the comparative example 1, the comparative example 2 and the example 1 is 57.3%, 50.4% and 21.1% of the content of the active ingredients of the juniper berry extract in the anti-hair-loss hair care essences before the test respectively. It can be seen that the effective components in the juniper berry essential oil have better permeability in the anti-hair loss and hair care essence prepared by the invention, can quickly enter the scalp, and can be effectively absorbed and utilized by hair follicles, so as to play the effective roles of the components. The prepared hair-care shampoo has excellent permeability, the permeability of the juniper berry extract is improved, the volatility of the active ingredients is reduced, the volatility of the juniper berry extract is reduced by combining physical barrier and chemical inhibition means, the contact absorption time of scalp and the active ingredients is prolonged, in addition, the active ingredients are solubilized by forming micro emulsion, and the carrier is formed by omega-3 fatty acid and vitamin A, so that the absorption of the scalp to the active ingredients is effectively promoted.

3. System stability testing

Respectively taking 10g of the essence prepared in the comparative examples 1 and 2 and the essence prepared by the invention at normal temperature, respectively filling the 10g of the essence into a centrifugal tube, and placing the centrifugal tube into a centrifugal machine for 1000 r.min, 2000 r.min, 3000 r.4000 r.min and 5000 r.min^-1The sample is centrifuged for 10min at the rotating speed, and the sample is taken out to observe whether the sample is layered or not. The test results are shown in table 2.

Table 2:

as can be seen from Table 2, in comparative example 1, sedimentation occurs at 2000rpm, sedimentation is obvious and layering occurs as the rotating speed increases, in comparative example 2, a small amount of sedimentation occurs at 3000rpm, and sedimentation increases and layering occurs as the centrifugal rotating speed increases, and the essence prepared by the invention does not have layering and sedimentation phenomena as the centrifugal rotating speed increases until 5000 rpm. The reason is that the effective components in the juniper berry essential oil are solubilized by the formation of the microemulsion, and are uniformly dispersed and effectively fixed in a colloidal structure along with the compatibility with the vitamin A in the process of forming a viscous colloid with the microorganism A, D and the seaweed gel, and the beeswax plays the role of a suspending agent in the microemulsion, so that the probability of sedimentation and delamination of the juniper berry essential oil is reduced.

4. Comparison of usage effects

10 men and women (the hair quality and the hair quantity are basically the same) of the same age group are selected, half of the men (5 men +5 women) use the anti-hair loss hair care essence prepared by the invention, the other half use the hair care essence prepared by the comparative example 2, the use frequency is the same, after the hair care essence is used for 3 months and 6 months respectively, relevant data such as scalp, hair quality and the like of a person to be tested are observed and detected, and the data are shown in table 3.

Table 3: the effect of the essence prepared by the invention and the comparative example is suitable for users.

After the formula hair-care essence prepared by the invention is used for 15 days, the hair is obviously smooth compared with the hair, the secretion of scalp grease is reduced, and the glossiness of hair is enhanced. When the hair follicle is detected for 3 months, the hair follicles growing hair in the distribution part begin to grow new hair, and new hair grows in the original hair follicles growing only 1 hair, so that each hair follicle has 2-3 hairs. From the above results, it can be seen that the hair loss prevention and care essence prepared by the present invention can effectively care the scalp, make the hair more warm in the hair follicles of the scalp by promoting the growth of hair follicles and simultaneously enhance the diameter of existing hair, and increase the toughness of the hair, thereby reducing hair loss and broken hair, and finally increase the amount of hair of a user and provide excellent hair quality.

Claims

1. The anti-hair-loss hair care essence is characterized in that: the essence comprises, by weight, 50 parts of a component A, 15-20 parts of a component B, 5-10 parts of a component C, 2.5-5 parts of a component D, 0.5-1.5 parts of sorbitan fatty acid ester, 1-1.5 parts of sucrose fatty acid ester, 0.5-1 part of a saponin extract and 0.5-2 parts of seaweed gel, and the balance of purified water is 100 parts, wherein the component A and the component B are mixed, the sorbitan fatty acid ester, the sucrose fatty acid ester and the saponin extract are added and stirred at a high speed to form a micro emulsion, the component D and the seaweed gel are added into the micro emulsion and stirred at a low speed, then the component C is added, and the purified water is added to 100 parts and stirred continuously; the component A is prepared by adding 1-2 parts of fructus cnidii, 2-3 parts of semen cuscutae, 1-3 parts of tea seed meal, 1-2 parts of fructus kochiae, 0.01-0.08 part of cordyceps sinensis, 1-3 parts of gallnut, 2-3 parts of ginger and 0.2-0.8 part of American ginseng into 40-50 parts of ethanol water solution with volume concentration of 50% for reflux extraction, the component B is prepared by 4-7 parts of juniper berry extract, 0.5-1 part of thyme essential oil, 1-2 parts of lavender essential oil, 0.5-1.2 parts of sweet orange oil, 1-1.5 parts of peppermint oil, 0.1-0.5 part of clove oil and 20 parts of ethanol water solution with volume concentration of 50%, the component C is prepared by 2-3 parts of beeswax, 1-3 parts of petrolatum, 1-2 parts of cane wax and 20 parts of ethanol water solution with volume concentration of 50%, and the component D is prepared by 0.5-2 parts of omega-3 fatty acid, 0.5-0.8 parts of vitamin A and 0.8-0.8 part of vitamin D, 0.4-1 part of folic acid, 0.5-1 part of lysine, 0.1-0.6 part of oyster extract and 10 parts of 50% ethanol aqueous solution.

2. The method for preparing the anti-hair loss and hair care essence according to claim 1, wherein: the preparation method comprises the steps of firstly preparing a juniper berry extract, mixing common cnidium fruit, south dodder seed, tea seed meal, belvedere fruit, cordyceps sinensis, Chinese gall, ginger and American ginseng, adding an ethanol water solution, heating, refluxing and extracting, adding medicinal-grade active carbon, stirring and filtering to form a component A, adding thyme essential oil, lavender essential oil, sweet orange oil, peppermint oil, clove oil and the juniper berry extract into the ethanol water solution, stirring and mixing uniformly to form a component B, adding beeswax, petrolatum and cane sugar wax into the ethanol water solution, heating and stirring to form a component C, adding omega-3 fatty acid, vitamin A, vitamin D, folic acid, lysine and the oyster extract into the ethanol water solution, and stirring at normal temperature to form a component D; mixing the component A and the component B, adding sorbitan fatty acid ester, sucrose fatty acid ester and saponin extract, stirring at a high speed to form a micro emulsion, simultaneously adding the component D and seaweed gel into the micro emulsion under low-speed stirring, then adding the component C, adding purified water to make up 100 parts, and continuously stirring for 30-50 min.

3. The method for preparing the anti-hair loss and hair care essence according to claim 2, wherein: the preparation method of the juniper berry extract specifically comprises the steps of cleaning and drying mature juniper berries, adding a mixture consisting of absolute ethyl alcohol and isopropyl ether according to a mass ratio of 1: 2-5 to form a mixed solution 1, heating and extracting in a nitrogen atmosphere, and filtering to obtain an extract solution 1; adding purified water and ethanol into the same juniper berries according to a ratio of 1: 1-2 to form a mixture 2, heating, performing reflux extraction, filtering to obtain an extract 2, mixing the extract 1 and the extract 2 to form a mixed extract, performing reduced pressure distillation, collecting a fraction 1, a fraction 2, a fraction 3 and a fraction 4 in sections, and mixing to form a juniper berry extract, namely, juniper berry essential oil.

4. The method for preparing the anti-hair loss and hair care essence according to claim 3, wherein: the extraction liquid 1 is specifically prepared by heating the mixed liquid 1 to 60-75 ℃, introducing nitrogen, extracting for 3-4 hours under the pressure of 1.0-1.2 MPa, then cooling to 5-10 ℃, decompressing, filtering and separating to obtain the extraction liquid 1.

5. The method for preparing the anti-hair loss and hair care essence according to any one of claims 3 or 4, wherein: the extraction liquid 2 is specifically prepared by heating the mixed liquid 2 to 100-110 ℃, performing reflux extraction for 5-6 h, then cooling to 20-30 ℃, and filtering and separating to obtain the extraction liquid 2.

6. The method for preparing the anti-hair loss and hair care essence according to any one of claims 3 to 5, wherein: and the step of collecting fractions in a segmented manner is to distill the mixed extract for 1 hour at the temperature of 30-40 ℃ and under the absolute pressure of 500-1000 Pa, then reduce the absolute pressure to 50Pa, and collect fraction 1.

7. The method for preparing the anti-hair loss and hair care essence according to claim 6, wherein: after the fraction 1 is collected, maintaining the absolute pressure at 30-50 Pa, raising the temperature to 60-100 ℃ at the speed of 0.5-1 ℃/min to collect the fraction 2, continuously raising the temperature to 110-150 ℃ to collect the fraction 3, and raising the temperature to 160-180 ℃ to collect the fraction 4.

8. The method for preparing the anti-hair loss and hair care essence according to claim 7, wherein: the juniper berry extract is formed by mixing fraction 1, fraction 2, fraction 3 and fraction 4 according to the mass ratio of 0.1-0.5: 0.2-0.5: 0.5-1: 0.3-0.5.

9. A preparation method of the hair loss preventing and protecting essence is characterized by comprising the following steps:

step 1, preparation of juniper berry extract

(1) Cleaning and drying mature juniper berries, adding a mixture consisting of absolute ethyl alcohol and isopropyl ether according to a mass ratio of 1: 2-5 to form a mixed solution 1, heating to 60-75 ℃ in a nitrogen atmosphere with the pressure of 1.0-1.2 MPa, extracting for 3-4 h, then cooling to 5-10 ℃, decompressing, filtering and separating to obtain an extract 1; adding the same juniper berries into a mixture of purified water and ethanol in a ratio of 1: 1-2 to form a mixed solution 2, heating to 100-110 ℃, performing reflux extraction for 5-6 hours, then cooling to 20-30 ℃, and filtering and separating to obtain an extract solution 2;

(2) mixing the extract 1 and the extract 2 to form a mixed extract, distilling for 1h at 30-40 ℃ and an absolute pressure of 500-1000 Pa, keeping the temperature unchanged, reducing the absolute pressure to 50Pa, collecting the fraction 1, then heating to 60-100 ℃ at a speed of 0.5-1/° C min, collecting the fraction 2, continuously heating to 110-150 ℃, collecting the fraction 3, continuously heating to 160-180 ℃ and collecting the fraction 4, and mixing the fraction 1, the fraction 2, the fraction 3 and the fraction 4 according to a mass ratio of 0.1-0.5: 0.2-0.5: 0.5-1: 0.3-0.5;

step 2, preparing essence

(1) Form the components

(2) mixing the components

Mixing 50 parts of the component A and 15-20 parts of the component B, adding 0.5-1.5 parts of sorbitan fatty acid ester, 1-1.5 parts of sucrose fatty acid ester and 0.5-1 part of Chinese honeylocust fruit extract, stirring at 1200-1500 rpm for 20-30 min to form a micro emulsion, adding 5-10 parts of the component C, 2.5-5 parts of the component D and 0.5-2 parts of seaweed gel, stirring at 30-50 rpm for 50-70 min, supplementing water until the total weight is 100 parts, and continuously stirring for 30-50 min.