Bath foam capable of clearing heat and decreasing internal heat and preparation method thereof

Abstract

The invention relates to the technical field of bubble bath liquid preparation, and particularly discloses a bubble bath liquid capable of clearing heat and decreasing internal heat and a preparation method thereof.The preparation method comprises the steps that fructus forsythiae, coptis chinensis roots, the root of kudzu vine, gleditsia sinensis seeds, honeysuckle, honeysuckle flowers, folium mori, andrographis paniculata leaves, mint, chrysanthemum and lophatherum gracile leaves are subjected to targeted pretreatment; the preparation method comprises the following steps: performing stepped synergistic extraction on pretreated raw materials, mixing an extracting solution, preparing a water phase, mixing and grinding borneol, ethanol, peppermint oil and a cyclodextrin inclusion compound into an oil phase, dynamically mixing the water phase and the oil phase to form an oil-in-water system, performing gradient concentration, staged sterilization and standing in sequence, and filling to obtain a finished product. The bath foam capable of clearing heat and decreasing internal heat is obtained. According to the method, the total extraction rate is increased by adopting synergistic pretreatment of composite enzymolysis and low-temperature freeze thawing activation, and meanwhile, the retention rate of various active ingredients is greatly increased by using a combined process of water extraction, alcohol extraction and ultrasonic extraction, so that the limitation of single solvent extraction is solved.

Description

TECHNICAL FIELD

[0001] The present application relates to the technical field of bath liquid, in particular to a bath liquid capable of clearing heat and reducing fire and a preparation method thereof. BACKGROUND

[0002] With the improvement of people's health consciousness, traditional Chinese medicine bath as a traditional health care method is widely used, especially in clearing heat and reducing fire, and is favored in skin soothing. Traditional heat-clearing bath liquid is mostly made of natural plants such as forsythia, coptis, and mint, relying on their cold nature to achieve the effect of clearing heat and reducing fire, cooling blood and detoxifying. Moreover, due to the natural ingredients and low irritation, it is suitable for daily care of all kinds of people.

[0003] However, the preparation method of such bath liquid in the prior art still has many deficiencies:

[0004] Firstly, the extraction rate of effective ingredients of raw materials is low. Most of the current processes use single water extraction or alcohol extraction method, without considering the differences in ingredient characteristics of different raw materials. For example, the water-soluble ingredients such as forsythia in forsythia and pueraria in pueraria, and the alkaloid ingredients such as berberine in coptis, have significant solubility differences under the same extraction conditions, and single solvent extraction cannot be considered; at the same time, the volatile oil components contained in honeysuckle and chrysanthemum are easily destroyed by high temperature extraction, resulting in a loss rate of heat-clearing active ingredients of more than 30%.

[0005] Secondly, the synergistic effect of raw materials is not fully exerted. The existing method mostly extracts all the raw materials after mixing, ignoring the mutual influence between the ingredients. For example, the saponin components in soapnut seeds have cleaning effect, but they are easy to form precipitate with alkaloids in coptis at high concentration, reducing the effect of both; the fat-soluble components such as borneol and mint oil are easy to separate or precipitate after conventional stirring and mixing due to poor compatibility with water phase, resulting in uneven heat-clearing and itching-relieving effect of the product.

[0006] Thirdly, the process stability and safety are insufficient. The traditional extraction process often uses high-temperature long-time decoction, which not only destroys the heat-sensitive flavonoids in mulberry leaves and lophatheri, but also increases the viscosity of the extraction liquid, making it difficult to filter later; the sterilization step mostly relies on single ultraviolet irradiation or high-temperature sterilization, the former is difficult to penetrate the thick liquid preparation, resulting in incomplete sterilization, and the latter further aggravates the degradation of effective ingredients, resulting in a shelf life of less than 3 months, and easy to cause skin irritation problems due to microbial residues.

[0007] Fourthly, the pretreatment method of raw materials is simple. The existing technology mostly uses direct crushing or whole material extraction for raw materials, without considering the hindering of plant cell wall to the dissolution of ingredients. For example, the cellulose, pectin and other components of forsythia, pueraria and other highly lignified raw materials form a dense structure, and the dissolution rate of effective ingredients in conventional extraction is less than 50%, which not only wastes raw materials, but also limits the heat-clearing effect of bath liquid.

[0008] Therefore, it is necessary to design a preparation method of a bubble bath liquid capable of clearing heat and reducing fire to solve the problems of low utilization rate of effective components, poor raw material synergy and insufficient stability in the existing bubble bath liquid preparation process. SUMMARY

[0009] Therefore, the present application provides a preparation method of a bubble bath liquid capable of clearing heat and reducing fire to solve the problems of low utilization rate of effective components, poor raw material synergy and insufficient stability in the existing bubble bath liquid preparation process.

[0010] In one aspect, the present application provides a preparation method of a bubble bath liquid capable of clearing heat and reducing fire, comprising the following preparation steps:

[0011] The forsythia, goldthread root, radix puerariae and soapnut seeds are crushed and then subjected to enzyme hydrolysis treatment respectively to obtain enzyme hydrolysis powder; the honeysuckle, honeysuckle flowers, mulberry leaves, andrographis leaves, peppermint, chrysanthemum and lophatheri leaves are subjected to low-temperature freeze-thaw activation treatment to obtain activated raw materials;

[0012] The activated raw materials, soapnut seed enzyme hydrolysis powder and forsythia enzyme hydrolysis powder are mixed and then water extraction is performed, and after filtration, a first extraction liquid and filter residue are obtained;

[0013] The filter residue and radix puerariae enzyme hydrolysis powder are mixed and then alcohol extraction is performed, and after filtration, a second extraction liquid is obtained;

[0014] Ethanol is added to the goldthread root enzyme hydrolysis powder, and low-temperature ultrasonic extraction is performed to obtain a third extraction liquid;

[0015] The first extraction liquid, second extraction liquid and third extraction liquid are stirred to obtain an aqueous phase base, ice is added to an ethanol solution and stirred until dissolved, then mixed with peppermint oil, and then cyclodextrin inclusion compound is added and ground to obtain an oil phase;

[0016] The oil phase is added dropwise to the aqueous phase, and at the same time, pulse stirring is started, and after the end, an oil-in-water system is obtained;

[0017] The oil-in-water system is subjected to gradient concentration and then sterilization treatment to obtain a material liquid, and after standing, the supernatant is taken for filling to obtain a bubble bath liquid capable of clearing heat and reducing fire.

[0018] Further, the enzyme hydrolysis treatment specifically comprises: 3% of a composite enzyme by mass is added to the crushed forsythia, goldthread root, radix puerariae and soapnut seeds, and enzyme hydrolysis is performed at 45°C and pH 4.5 for 30 minutes, and then 80°C water bath inactivation is performed for 10 minutes.

[0019] Further, the low-temperature freeze-thaw activation treatment specifically comprises: freezing honeysuckle, honeysuckle flowers, mulberry leaves, andrographis leaves, peppermint, chrysanthemum, and lophatherum gracile leaves at a temperature of-15 DEG C for 2 hours, and immediately spraying with 30 DEG C warm water for 3 minutes after taking out, and repeating 2 times.

[0020] Further, the water extraction specifically comprises: adding 8 times of water in mass to the mixed activated raw materials, the gleditsia sinensis seed enzymatic powder and the forsythia suspense enzymatic powder, boiling for 10 minutes first, and then reducing the temperature to 50 DEG C for 90 minutes of heat preservation extraction.

[0021] Further, the alcohol extraction specifically comprises: adding 6 times of 50% ethanol in mass to the mixed filtrate and the puerariae radix enzymatic powder, and carrying out cyclic reflux at 60 DEG C, refluxing once every 30 minutes, a total of 3 times, and vacuumizing to-0.06 MPa for 5 minutes after each refluxing.

[0022] Further, the low-temperature ultrasonic extraction is carried out at a temperature of 25 DEG C, an ultrasonic power of 200 W, and an ultrasonic mode of pausing for 2 seconds every 3 seconds of working, and a total extraction time of 15 minutes.

[0023] Further, the pulse stirring specifically comprises: stirring at 60 r / min for 30 seconds, pausing for 10 seconds, stirring at 120 r / min for 30 seconds, pausing for 10 seconds, and repeating the step for 40 minutes.

[0024] Further, the gradient concentration specifically comprises: first concentrating the oil-in-water system at 45 DEG C under reduced pressure to 1 / 3 of the original volume, and then continuing to concentrate at 60 DEG C to a relative density of 1.08.

[0025] Further, the sterilization treatment specifically comprises: first treating with a microwave of 300 W for 2 minutes, pausing for 10 seconds every 20 seconds of treatment, and then irradiating with ultraviolet rays of 254 nm for 20 minutes.

[0026] On the other hand, the application also provides a bubble bath liquid capable of clearing heat and reducing fire.

[0027] Compared with the prior art, the application has the beneficial effects that:

[0028] 1. The application adopts the synergistic pretreatment of composite enzymolysis and low-temperature freeze-thaw activation: the composite enzyme can destroy the cell wall structure of the lignified raw materials such as forsythia suspense and puerariae radix, and cooperate with the physical wall-breaking effect of freeze-thaw, so that the cell gap of the raw materials such as honeysuckle and chrysanthemum is expanded, and the total extraction rate is improved. Meanwhile, the combination process of water extraction, alcohol extraction and ultrasonic extraction is used, which is respectively matched with the solubility characteristics of water-soluble ingredients (forrestoside), alcohol-soluble ingredients (puerarin) and alkaloid ingredients (berberine), so that the retention rate of various active ingredients is greatly improved, and the limitation of single solvent extraction is solved.

[0029] 2、The application realizes precise compounding by feeding the enzyme hydrolyzed powder in stages, the enzyme hydrolyzed powder of forsythia and the enzyme hydrolyzed powder of soapnut seed are added in the first water extraction, the heat clearing activity is enhanced by the synergistic effect of forsythoside and saponin; the enzyme hydrolyzed powder of pueraria is added in the second alcohol extraction, the precipitation of the alkaloid of rhizoma coptidis and the enzyme hydrolyzed powder of pueraria in the water phase is avoided; meanwhile, the dispersity of the borneol and the peppermint oil is improved by the cyclodextrin inclusion technology combined with pulse stirring, the stratification problem of the fat-soluble ingredients is solved, and the uniform release of the heat clearing and itching relieving effect is ensured.

[0030] 3、The application can reduce the degradation of heat-sensitive components such as mulberry leaf flavonoids and puerarin by gradient concentration, and improve the retention rate. BRIEF DESCRIPTION OF DRAWINGS

[0031] Various other advantages and benefits will become apparent to those of ordinary skill in the art upon reading the following detailed description of the preferred embodiments with reference made to the accompanying drawings. The drawings are for purposes of illustration only and are not intended to be limiting, of the application. Like reference numerals have been used wherever possible throughout the drawings to refer to like parts. In the drawings:

[0032] Figure 1 The preparation method flow chart of the bubble bath liquid capable of clearing heat and reducing fire provided by the embodiment of the application. DETAILED DESCRIPTION

[0033] The technical solutions in the embodiments of the application will be apparently and completely described below with reference to the drawings in the embodiments of the application. Obviously, the described embodiments are only part of the embodiments of the application, rather than all the embodiments of the application. Based on the embodiments in the application, all other embodiments obtained by those of ordinary skill in the art without creative labor fall within the protection scope of the application.

[0034] In the description of the application, it should be understood that the terms "center", "upper", "lower", "front", "back", "left", "right", "vertical", "horizontal", "top", "bottom", "inner", "outer" and the like indicate the orientation or positional relationship based on the orientation or positional relationship shown in the drawings, and are only for the purpose of facilitating the description of the application and simplifying the description, and therefore cannot be understood as indicating or implying that the device or element referred to must have a particular orientation, be constructed and operated in a particular orientation, and therefore cannot be understood as limiting the application.

[0035] The terms "first", "second" are only for the purpose of description, and cannot be understood as indicating or implying relative importance or implicitly indicating the number of the indicated technical features. Therefore, the features defined as "first", "second" can explicitly or implicitly include one or more features. In the description of the application, unless otherwise specified, the meaning of "multiple" is two or more.

[0036] In the description of the present application, it should be noted that unless otherwise explicitly specified and limited, the terms "mounting", "connection", "connecting" should be understood in a broad sense, for example, can be fixed connection, can also be detachable connection, or integral connection; can be mechanical connection, can also be electrical connection; can be directly connected, can also be indirectly connected through an intermediate medium, can be the communication inside two elements. For those skilled in the art, the specific meaning of the above terms in the present application can be understood according to the specific circumstances.

[0037] In one aspect, as Figure 1 shown, in some embodiments of the present application, a preparation method of a bubble bath liquid for clearing heat and reducing fire, comprising the following preparation steps:

[0038] After the forsythia, goldthread root, radix puerariae, and soapberry seeds are crushed, enzyme hydrolysis treatment is carried out respectively to obtain enzyme hydrolysis powder; the honeysuckle, honeysuckle flowers, mulberry leaves, and andrographis leaves, mint, chrysanthemum, and lophatheri leaves are subjected to low-temperature freeze-thaw activation treatment to obtain activated raw materials;

[0039] After the activated raw materials, the soapberry seed enzyme hydrolysis powder, and the forsythia enzyme hydrolysis powder are mixed, water is added for water extraction, and after filtration, a first extraction liquid and a filter residue are obtained;

[0040] After the filter residue and the radix puerariae enzyme hydrolysis powder are mixed, ethanol is added for alcohol extraction, and after filtration, a second extraction liquid is obtained;

[0041] Ethanol is added to the goldthread root enzyme hydrolysis powder for low-temperature ultrasonic extraction to obtain a third extraction liquid;

[0042] The first extraction liquid, the second extraction liquid, and the third extraction liquid are stirred to obtain an aqueous phase base, menthol is added to an ethanol solution, stirred until dissolved, mixed with mint oil, and then cyclodextrin inclusion compound is added, ground to obtain an oil phase;

[0043] The oil phase is added dropwise to the aqueous phase, and at the same time, pulse stirring is started, and after the end, an oil-in-water system is obtained;

[0044] After the oil-in-water system is subjected to gradient concentration, sterilization treatment is carried out to obtain a material liquid, the material liquid is left to stand, the supernatant is taken for filling to obtain a bubble bath liquid for clearing heat and reducing fire.

[0045] Specifically, the use amount of the forsythia, honeysuckle, honeysuckle flowers, goldthread root, menthol, mulberry leaves, radix puerariae, andrographis leaves, mint, chrysanthemum, lophatheri leaves, mint oil, and soapberry seeds is (in mass fraction):

[0046] Forintia 5-10 parts, honeysuckle 5-10 parts, honeysuckle flower 3-8 parts, Rhizoma Coptidis 3-8 parts, borneol 0.5-1.5 parts, mulberry leaves 3-8 parts, radix puerariae 3-8 parts, Andrographis Herba 8-15 parts, mint 3-8 parts, chrysanthemum 3-8 parts, lophatheri 3-8 parts, peppermint oil 0.5-1.5 parts, and soap nut 0.5-1.5 parts

[0047] Preferably, Forintia 8 parts, honeysuckle 8 parts, honeysuckle flower 5 parts, Rhizoma Coptidis 5 parts, borneol 1 part, mulberry leaves 5 parts, radix puerariae 5 parts, Andrographis Herba 10 parts, mint 5 parts, chrysanthemum 5 parts, lophatheri 5 parts, peppermint oil 1 part, and soap nut 1 part.

[0048] Specifically, the Forintia, Rhizoma Coptidis, radix puerariae and soap nut are crushed to 20-40 mesh.

[0049] Specifically, the cellulase: pectinase in the complex enzyme is 1:1.

[0050] Specifically, when the ethanol is added to the Rhizoma Coptidis enzymolysis powder for low-temperature ultrasonic extraction, the ethanol is 75% ethanol, and the mass of the ethanol is 3 times the mass of the Rhizoma Coptidis enzymolysis powder.

[0051] Specifically, when the first extract, the second extract and the third extract are stirred to obtain the water phase base, the stirring speed is 30 r / min and the stirring time is 20 minutes.

[0052] Specifically, when the borneol is added to the ethanol solution and stirred to dissolve and then mixed with the peppermint oil, the ethanol solution is 95% ethanol, and the mass of the ethanol solution is 8 times the mass of the borneol.

[0053] Specifically, the β-cyclodextrin: water in the cyclodextrin inclusion compound is 1:5.

[0054] Specifically, when the oil phase is added dropwise into the water phase, the oil phase is added dropwise into the water phase at a speed of 1 drop per second.

[0055] Specifically, when standing and filling, the standing is carried out at 25°C for 24 hours, the filling is carried out in a sterile environment, the temperature of the supernatant is controlled to be 38-40°C, and the filling is carried out.

[0056] It can be understood that the addition of peppermint oil has the following effects:

[0057] 1. Treatment of cold: Peppermint oil can be inhaled by the respiratory tract through the steam method, promote the body to sweat, and help to eliminate inflammation related to the respiratory tract, thereby relieving the symptoms of cold.

[0058] 2. Anti-inflammatory and analgesic: Peppermint oil has the effects of anti-inflammatory and analgesic, and can be directly used for the treatment of symptoms such as headache, migraine and toothache to relieve pain.

[0059] 3. Relieving pain in throat: Peppermint oil can relieve the pain in throat.

[0060] 4. Dispelling wind and clearing heat: Peppermint oil can dispel wind and clear heat, and has certain therapeutic effect on symptoms such as exogenous wind-heat, headache and red eyes, and sore throat.

[0061] It can be understood that the present application adopts the synergistic pretreatment of composite enzymolysis and low-temperature freeze-thaw activation: the composite enzyme can destroy the cell wall structure of the lignified raw materials such as forsythia and pueraria, and cooperate with the physical wall-breaking effect of freeze-thaw to expand the intercellular space of the raw materials such as honeysuckle and chrysanthemum, thereby improving the total extraction. Meanwhile, the combination process of water extraction, alcohol extraction and ultrasonic extraction is used to adapt to the solubility characteristics of water-soluble ingredients (forysthia glycoside), alcohol-soluble ingredients (puerarin) and alkaloid ingredients (berberine), so that the retention rate of various active ingredients is greatly improved, and the limitations of single solvent extraction are solved.

[0062] It can be understood that the present application realizes precise compounding by adding enzyme hydrolysis powder in stages, the first water extraction adds forsythia enzyme hydrolysis powder and soapnut seed enzyme hydrolysis powder, and the synergistic effect of forysthia glycoside and saponin is used to enhance the heat-clearing activity; the second alcohol extraction adds pueraria enzyme hydrolysis powder to avoid the precipitation of pueraria and alkaloids in water; meanwhile, through the cyclodextrin inclusion technology combined with pulse stirring, the dispersity of borneol and peppermint oil is improved, the stratification problem of fat-soluble ingredients is solved, and the uniform release of heat-clearing and itching-relieving effect is ensured.

[0063] It can be understood that the present application can reduce the degradation of heat-sensitive components such as mulberry leaf flavonoids and timosaponin through gradient concentration, and improve the retention rate.

[0064] In some embodiments of the present application, the enzyme hydrolysis treatment is specifically: 3% by mass of composite enzyme is added to the crushed forsythia, rhizoma coptidis, pueraria and soapnut seed, respectively, and enzyme hydrolysis is carried out at 45℃ and pH 4.5 for 30 minutes, and then 80℃ water bath inactivation for 10 minutes.

[0065] Specifically, 3% by mass of composite enzyme (cellulase and pectinase) is added, and enzyme hydrolysis is carried out at 45℃ (optimal temperature of enzyme activity) and pH 4.5 (optimal pH of enzyme reaction) for 30 minutes, which can specifically decompose the cellulose and pectin components in the cell wall of the raw materials, break the package of effective components by lignified structure, and improve the dissolution of active substances such as forysthia glycoside, berberine and puerarin; and then 80℃ water bath inactivation for 10 minutes, which can quickly terminate the enzyme activity, prevent the degradation of components caused by excessive enzyme hydrolysis, and further loosen the cell structure by using short-time high temperature, thereby creating favorable conditions for the subsequent extraction steps, and finally realizing the dual improvement of the utilization rate and stability of the effective components of the raw materials.

[0066] In some embodiments of the present application, the low-temperature freeze-thaw activation treatment specifically comprises: freezing Lonicera japonica, Lonicera japonica flowers, mulberry leaves, Andrographis herb, Mentha haplocalyx, Chrysanthemum morifolium and Agastache rugosa leaves at a temperature of-15°C for 2 hours, immediately spraying with warm water at 30°C for 3 minutes after taking out, and repeating 2 times.

[0067] Specifically, Lonicera japonica, Lonicera japonica flowers, mulberry leaves, Andrographis herb, Mentha haplocalyx, Chrysanthemum morifolium and Agastache rugosa leaves are frozen at a temperature of-15°C for 2 hours, immediately sprayed with warm water at 30°C for 3 minutes after taking out, and then frozen at a temperature of-15°C for 2 hours again, immediately sprayed with warm water at 30°C for 3 minutes after taking out.

[0068] It can be understood that the “low-temperature freeze-thaw activation” treatment of Lonicera japonica, Lonicera japonica flowers, mulberry leaves, Andrographis herb, Mentha haplocalyx, Chrysanthemum morifolium and Agastache rugosa leaves expands the intracellular water crystallization by freezing at-15°C, destroys the integrity of the cell wall, and then forms a temperature shock by spraying with warm water at 30°C, further expanding the intercellular space and cell membrane permeability. Repeating 2 times can strengthen the physical wall-breaking effect, which not only avoids the destruction of heat-sensitive active ingredients such as menthol and chrysosplenol D by high-temperature treatment, but also significantly improves the dissolution rate of flavonoids, volatile oils and other heat-clearing ingredients during subsequent extraction. At the same time, the mild physical treatment method retains the natural activity of the raw materials, avoids the pollution of ingredients caused by the intervention of chemical reagents, and forms a synergy with the subsequent extraction process, laying a foundation for the heat-clearing effect and mildness of the bath liquid.

[0069] In some embodiments of the present application, the water extraction specifically comprises: adding 8 times the mass of water to the mixed activated raw materials, soapnut seed enzymatic powder and forsythia enzymatic powder, boiling for 10 minutes first, and then reducing the temperature to 50°C for 90 minutes of extraction.

[0070] Specifically, the water is preferably deionized water, and the water extraction is manually stirred with a bamboo sieve every 15 minutes.

[0071] It can be understood that the freeze-thawed complete raw material is mixed with forsythia enzyme powder and soapberry seed enzyme powder for extraction, the natural active structure retained by the freeze-thawed raw material and the small molecule state of the enzyme powder can form complementation, the forsythia in the forsythia enzyme powder can be quickly dissolved to play a core role of clearing heat, and the saponin component in the soapberry seed enzyme powder can reduce the surface tension of the system to promote the dissolution of other components; the addition of 8 times the mass of deionized water can not only ensure sufficient solvent, but also avoid the increase of subsequent concentration energy consumption caused by excessive solvent. In the "boiling first and then warming" extraction method, 10 minutes of boiling can quickly destroy the cell wall barrier of the raw material, inactivate endogenous enzymes and preliminarily sterilize, and then the temperature is lowered to 50℃ for extraction, which can avoid the degradation of heat-sensitive components such as menthol and chrysin, while providing a suitable dissolution temperature for flavonoids and polysaccharides; the bamboo sieve is manually stirred every 15 minutes, which can break the concentration gradient on the surface of the raw material through gentle mechanical action, promote the uniform diffusion of the components, and avoid the excessive damage of mechanical stirring to the fragile structure of the raw material, so as to finally realize the balance between high retention rate of effective components and extraction efficiency, and lay a foundation for the clearing heat efficiency and stability of the bath liquid.

[0072] In some embodiments of the present application, the alcohol extraction is specifically: 6 times the mass of 50% ethanol is added to the mixed filtrate and the kudzu enzyme powder, and the system is subjected to cyclic reflux at 60℃, refluxing once every 30 minutes, a total of 3 times, and vacuumizing to-0.06MPa for 5 minutes after each reflux.

[0073] Specifically, the 50% ethanol used in the alcohol extraction also contains 0.1% acetic acid.

[0074] It can be understood that the addition of kudzu enzyme powder to the residue after water extraction can realize the secondary efficient utilization of components through the synergistic effect of alcohol-soluble components such as puerarin in kudzu and residual active substances in the residue; 6 times the mass of 50% ethanol (containing 0.1% acetic acid) provides a suitable polar environment for the system, and acetic acid can adjust the pH to weakly acidic to promote the dissolution of components such as alkaloids of coptis rhizome and puerarin, and avoid the damage of high-concentration ethanol to the components. The temperature of 60℃ is suitable for the dissolution characteristics of alcohol-soluble components, which can ensure the dissolution efficiency and reduce the loss of volatile oil. The 3 times of cyclic reflux can continuously update the contact interface between the solvent and the residue, and fully extract the residual components; vacuumizing to-0.06MPa after each reflux can use the negative pressure difference to expand the intercellular space of the residue, enhance the penetration of ethanol, and at the same time remove low-boiling-point impurities through flash evaporation to improve the purity of the extract. This process not only solves the problem of raw material waste caused by the traditional disposal of residue, but also specifically strengthens the extraction of alcohol-soluble heat-clearing components, realizes the dual improvement of resource utilization rate and retention rate of effective components.

[0075] In some embodiments of the present application, the temperature of the low-temperature ultrasonic extraction is 25℃, the ultrasonic power is 200W, the ultrasonic mode is 3 seconds of work and 2 seconds of pause, and the total extraction time is 15 minutes.

[0076] Specifically, the enzymatic powder of Coptis root is added into 3 times of 75% ethanol, and then treated with 200W ultrasonic at 25℃ for 3 seconds and 2 seconds intermittently. After 15 minutes of treatment, filtration is performed.

[0077] It can be understood that, the enzymatic powder of Coptis root is treated alone, so that the alkaloids such as berberine contained in the powder and the saponins in other raw materials are prevented from forming a precipitate, and the purity of the active ingredients is ensured; 75% ethanol is the optimal solvent for alkaloids of Coptis root, and can improve the dissolution rate of berberine; the low temperature environment of 25℃ can prevent the degradation of alkaloids caused by high temperature, and the intermittent treatment with 200W ultrasonic can break the particle aggregation of the enzymatic powder through the cavitation effect of ultrasonic, and accelerate the penetration of the solvent, and can also prevent the destruction of the stability of the components caused by local high temperature generated by continuous ultrasonic, and the treatment time of 15 minutes can ensure sufficient extraction while reducing energy consumption; the solvent dosage of 3 times of the mass of the enzymatic powder can precisely match the adsorption characteristics of the enzymatic powder, so that the solvent is not wasted, and the active ingredients are fully dissolved. The process realizes the efficient and directional extraction of the core heat-clearing ingredients of Coptis root, and provides ingredient support for the heat-clearing and detoxifying effect of the bath liquid.

[0078] In some embodiments of the present application, the pulse stirring is specifically: stirring at 60r / min for 30 seconds, pausing for 10 seconds, stirring at 120r / min for 30 seconds, pausing for 10 seconds, and repeating this step for 40 minutes.

[0079] It can be understood that, the dynamic and alternating mechanical action realizes the efficient fusion of the oil phase (ice ethanol solution, peppermint oil) and the water phase: the low speed (60r / min) stage can let the oil phase droplets be initially dispersed in the water phase, and avoid the aggregation of the droplets caused by direct impact of high speed; the high speed (120r / min) stage can further refine the droplets to micron level through stronger shear force, and improve the dispersion uniformity; the alternating rhythm of 30 seconds of stirring and 10 seconds of pausing can break the interfacial tension by using stirring kinetic energy, and can also let the system naturally balance through molecular diffusion during the pausing period, so as to reduce the influence of the bubbles generated by continuous stirring on the stability of the emulsion. This dynamic regulation mode improves the dispersion coefficient of the fat-soluble ingredients compared with the conventional uniform stirring, and avoids the damage to the heat-sensitive ingredients caused by excessive mechanical shear, so as to ensure the uniform release of the heat-clearing ingredients of the bath liquid, and improve the consistency of the cooling and soothing experience during use.

[0080] In some embodiments of the present application, the gradient concentration is specifically: first, the oil-in-water system is concentrated under reduced pressure at 45℃ to 1 / 3 of the original volume, and then the temperature is increased to 60℃ to continue the concentration to a relative density of 1.08.

[0081] It can be understood that, first, the solution is concentrated at 45°C under reduced pressure to 1 / 3 of the original volume, the boiling point of the solution is reduced in a reduced pressure environment, and a large amount of free water is quickly removed under low temperature conditions, so that the heat-sensitive active ingredients such as forsythoside and menthol can be maximally preserved; then, the temperature is increased to 60°C and the concentration is continued to 1.08 of the relative density, at this time, because the volume of the solution has been greatly reduced, moderate temperature increase can speed up the evaporation of the remaining water, improve the concentration efficiency, and the 60°C temperature will not cause damage to the components with strong stability such as berberine and puerarin. This gradient reduced pressure concentration process not only avoids the degradation of heat-sensitive components caused by single high temperature, but also solves the problem of low concentration efficiency under low temperature all the time. The concentration liquid obtained finally has uniform active ingredient concentration and stable relative density of 1.08, which lays a foundation for the consistency of efficacy and the extension of shelf life of the subsequent bath liquid.

[0082] In some embodiments of the present application, the sterilization treatment is specifically: first, 300W microwave treatment for 2 minutes, 10 seconds pause every 20 seconds, and then 254nm ultraviolet irradiation for 20 minutes.

[0083] Specifically, first, 300W microwave treatment for 2 minutes, 10 seconds pause every 20 seconds, and then transfer into an ultraviolet sterilization box for 20 minutes of 254nm ultraviolet irradiation.

[0084] It can be understood that, first, 300W microwave intermittent treatment is used to penetrate the liquid deep layer by using the heat effect and non-thermal effect of microwave, quickly kill the bacterial spores and fungi hidden in the inside of the concentrated liquid, and the intermittent operation can avoid the damage to heat-sensitive components such as forsythoside and menthol caused by local high temperature generated by continuous microwave; then, transfer into a 254nm ultraviolet sterilization box for 20 minutes of irradiation, use the damage effect of ultraviolet on microbial DNA to kill the residual microorganisms on the surface and in suspension of the solution, and make up for the defect that microwave is not thorough in killing the microorganisms in the shallow layer. This synergistic process of “microwave deep layer sterilization + ultraviolet surface layer sterilization” can greatly improve the thoroughness of sterilization, and greatly reduce the damage rate of active ingredients, which not only ensures the microbial safety of the bath liquid, but also maintains its heat-clearing activity.

[0085] On the other hand, in some embodiments of the present application, the present application also provides a bath liquid capable of clearing heat and reducing fire.

[0086] Embodiment 1

[0087] S1, take forsythia 5 parts, coptis root 3 parts, pueraria 3 parts and soapnut seed 0.5 parts, crush them to 20-40 mesh, then add 3% of the mass of each of the composite enzyme, and enzymatically hydrolyze at 45°C and pH 4.5 for 30 minutes, and then inactivate in a water bath at 80°C for 10 minutes to obtain an enzymatic hydrolysis powder;

[0088] S2, freeze Lonicera japonica 5 parts, honeysuckle flower 3 parts, mulberry leaf 3 parts, Andrographis herb 8 parts, mint 3 parts, chrysanthemum 3 parts and lophatherum leaf 3 parts at a temperature of-15℃ for 2 hours, immediately after taking out, spray with warm water at 30℃ for 3 minutes, after the end, again freeze them at a temperature of-15℃ for 2 hours, immediately after taking out, spray with warm water at 30℃ for 3 minutes, to obtain the activated raw materials;

[0089] S3, mix the activated raw materials with forsythia enzymatic powder and soapnut seed enzymatic powder, add 8 times the mass of deionized water, first boil for 10 minutes, cool to 50℃, extract for 90 minutes, manually stir with bamboo sieve every 15 minutes, filter to obtain the first extract and filter residue;

[0090] S4, mix the filter residue with the kudzu vine enzymatic powder, add 6 times the mass of 50% ethanol containing 0.1% acetic acid, carry out cyclic reflux at 60℃, reflux every 30 minutes, a total of 3 times, after each reflux, vacuumize to-0.06MPa for 5 minutes, after the end, filter to obtain the second extract;

[0091] S5, add 3 times the mass of 75% ethanol to the Coptis chinensis root enzymatic powder, use 200W ultrasonic wave at 25℃, with the ultrasonic mode of 3 seconds working and 2 seconds pausing, extract for 15 minutes, filter to obtain the third extract;

[0092] S6, mix the first extract, the second extract and the third extract, stir at a speed of 30r / min for 20 minutes to obtain the water phase base, mix borneol 0.5 parts and mint oil 0.5 parts, add 5 times the mass of cyclodextrin inclusion compound, grind until the oil phase is formed;

[0093] S7, drop the oil phase into the water phase at a speed of 1 drop / second, at the same time, start the pulse stirring, stir at a speed of 60r / min for 30 seconds, pause for 10 seconds, then stir at a speed of 120r / min for 30 seconds, pause for 10 seconds, repeat this step for 40 minutes, after the end, obtain the oil-in-water system;

[0094] S8, first concentrate the oil-in-water system at 45℃ under reduced pressure to 1 / 3 of the original volume, then heat to 60℃ to continue concentrating to a relative density of 1.08, then first treat the concentrated solution with 300W microwave for 2 minutes, during which, pause for 10 seconds every 20 seconds, then transfer into the ultraviolet sterilization box, irradiate with ultraviolet rays at a wavelength of 254nm for 20 minutes, after the end, stand at 25℃ for 24 hours, take the supernatant, adjust the temperature of the supernatant to between 38-40℃, carry out filling in a sterile environment to obtain the bubble bath liquid capable of clearing heat and reducing fire.

[0095] Example 2

[0096] S1, take forsythia 8 parts, rhizoma coptidis 5 parts, radix puerariae 5 parts and gleditsiae 1 part, crush to 20-40 mesh, then add 3% of the mass of composite enzyme, enzymolysis at 45℃ and pH 4.5 for 30 minutes, then inactivate at 80℃ water bath for 10 minutes, to obtain enzyme hydrolysis powder;

[0097] S2, take honeysuckle 8 parts, honeysuckle flower 5 parts, mulberry leaf 5 parts, andrographis 10 parts, mint 5 parts, chrysanthemum 5 parts and lophatheri 5 parts, freeze at-15℃ for 2 hours, then immediately spray with 30℃ warm water for 3 minutes, then freeze at-15℃ for 2 hours again, then immediately spray with 30℃ warm water for 3 minutes, to obtain activated raw materials;

[0098] S3, mix the activated raw materials with forsythia enzyme hydrolysis powder and gleditsiae enzyme hydrolysis powder, add 8 times the mass of deionized water, boil for 10 minutes, then cool to 50℃ and extract for 90 minutes, manually stir with bamboo sieve every 15 minutes, filter to obtain first extract and filter residue;

[0099] S4, mix the filter residue with radix puerariae enzyme hydrolysis powder, then add 6 times the mass of 50% ethanol containing 0.1% acetic acid, perform cyclic reflux at 60℃, reflux every 30 minutes for a total of 3 times, vacuum to-0.06MPa for 5 minutes after each reflux, then filter to obtain second extract;

[0100] S5, add 3 times the mass of 75% ethanol to the rhizoma coptidis enzyme hydrolysis powder, use 200W ultrasonic at 25℃, ultrasonic mode of 3 seconds working and 2 seconds pause, extract for 15 minutes, filter to obtain third extract;

[0101] S6, mix the first extract, second extract and third extract, stir at 30r / min for 20 minutes to obtain water phase base, mix borneol 1 part and mint oil 1 part, add 5 times the mass of cyclodextrin inclusion compound, grind until oil phase is formed;

[0102] S7, drop the oil phase into the water phase at a speed of 1 drop / second, start pulse stirring at the same time, stir at 60r / min for 30 seconds, pause for 10 seconds, then stir at 120r / min for 30 seconds, pause for 10 seconds, repeat this step for 40 minutes, then obtain oil-in-water system;

[0103] S8, the oil-in-water system is first concentrated at 45℃ under reduced pressure to 1 / 3 of the original volume, then warmed to 60℃ and concentrated to a relative density of 1.08, then the concentrated solution is first treated with a 300W microwave for 2 minutes, during which it is stopped every 20 seconds for 10 seconds, then transferred into a UV sterilization box and irradiated with UV light at a wavelength of 254nm for 20 minutes, after which it is left to stand at 25℃ for 24 hours, the supernatant is taken, the temperature of the supernatant is adjusted to between 38-40℃, and the filling is carried out in a sterile environment to obtain a bubble bath liquid that can clear heat and reduce fire.

[0104] Example 3

[0105] S1, take forsythia 10 parts, goldthread root 8 parts, kudzu root 8 parts, and soapnut 1.5 parts, crush to 20-40 mesh, then add 3% of the mass of each of the composite enzymes, and enzymatically hydrolyze at 45℃ and pH 4.5 for 30 minutes, then inactivate by water bath at 80℃ for 10 minutes to obtain enzymatic hydrolysis powder;

[0106] S2, freeze honeysuckle 10 parts, honeysuckle flower 8 parts, mulberry leaf 5 parts, andrographis leaf 15 parts, mint 8 parts, chrysanthemum 8 parts, and lophatherum leaf 8 parts at a temperature of -15℃ for 2 hours, immediately after taking them out, spray with warm water at 30℃ for 3 minutes, then again freeze them at a temperature of -15℃ for 2 hours, immediately after taking them out, spray with warm water at 30℃ for 3 minutes to obtain activated raw materials;

[0107] S3, mix the activated raw materials with the forsythia enzymatic hydrolysis powder and the soapnut enzymatic hydrolysis powder, add 8 times the mass of deionized water, and first boil for 10 minutes, then reduce the temperature to 50℃ and keep it for 90 minutes, manually stir every 15 minutes with a bamboo sieve, filter to obtain the first extract and the filter residue;

[0108] S4, mix the filter residue with the kudzu root enzymatic hydrolysis powder, then add 6 times the mass of 50% ethanol containing 0.1% acetic acid, and perform cyclic reflux at 60℃, reflux every 30 minutes for a total of 3 times, vacuumize to -0.06MPa for 5 minutes after each reflux, then filter to obtain the second extract;

[0109] S5, add 3 times the mass of 75% ethanol to the goldthread root enzymatic hydrolysis powder, and use 200W ultrasonic waves at an ultrasonic mode of 3 seconds of work and 2 seconds of pause every 3 seconds to extract for 15 minutes at 25℃, then filter to obtain the third extract;

[0110] S6, mix the first extract, the second extract, and the third extract, and stir at a speed of 30r / min for 20 minutes to obtain the water phase base, mix borneol 1.5 parts and mint oil 1.5 parts, add 5 times the mass of cyclodextrin inclusion compound to them, and grind until an oil phase is formed;

[0111] S7, the oil phase is dropped into the water phase at a speed of 1 drop per second, while the pulse stirring is started, stirring at 60 r / min for 30 seconds, pausing for 10 seconds, stirring at 120 r / min for 30 seconds, pausing for 10 seconds, repeating this step for 40 minutes, after which an oil-in-water system is obtained;

[0112] S8, the oil-in-water system is first concentrated at 45°C under reduced pressure to 1 / 3 of the original volume, then warmed to 60°C and continued to concentrate to a relative density of 1.08, then the concentrated solution is first treated with a microwave of 300W for 2 minutes, during which it is stopped for 10 seconds every 20 seconds, then transferred into a ultraviolet sterilization box and irradiated with ultraviolet light of wavelength 254nm for 20 minutes, after which it is left to stand at 25°C for 24 hours, the supernatant is taken, the temperature of the supernatant is adjusted to between 38-40°C, and the filling is carried out in a sterile environment to obtain a bubble bath liquid that can clear heat and reduce fire.

[0113] The above only describes the preferred embodiments of the present application, and it should be noted that for those skilled in the art, without departing from the principles of the present application, a number of improvements and refinements can be made, and these improvements and refinements should also be considered within the scope of protection of the present application.

Claims

1. A method for preparing a bubble bath liquid capable of clearing heat and reducing fire, characterized in that, The preparation method comprises the following steps: The forsythia, rhizoma coptidis, radix puerariae and gleditsiae sinensis seeds are crushed and then subjected to enzymatic hydrolysis to obtain enzymatic hydrolysis powder; the honeysuckle, honeysuckle flowers, mulberry leaves, andrographis leaves, mint, chrysanthemum and lophatheri leaves are subjected to low-temperature freeze-thaw activation to obtain activated raw materials; The activated raw materials, the gleditsiae sinensis seed enzymatic hydrolysis powder and the forsythia enzymatic hydrolysis powder are mixed and then water is added for water extraction, and then filtration is performed to obtain a first extraction liquid and a filter residue; The filter residue and the radix puerariae enzymatic hydrolysis powder are mixed and then ethanol is added for alcohol extraction, and then filtration is performed to obtain a second extraction liquid; Ethanol is added to the rhizoma coptidis enzymatic hydrolysis powder for low-temperature ultrasonic extraction to obtain a third extraction liquid; The first extraction liquid, the second extraction liquid and the third extraction liquid are stirred to obtain an aqueous phase base, ice is added to ethanol solution and stirred until dissolved, then mixed with mint oil, and then cyclodextrin inclusion compound is added and ground to obtain an oil phase; The oil phase is added dropwise to the aqueous phase, and pulse stirring is started at the same time, and then the process is ended to obtain an oil-in-water system; The oil-in-water system is subjected to gradient concentration and then sterilization treatment to obtain a liquid, and then the liquid is left to stand, and the supernatant is taken for filling to obtain a bubble bath liquid capable of clearing heat and reducing fire.

2. The preparation method of the bubble bath liquid capable of clearing heat and reducing fire according to claim 1, wherein the enzymatic hydrolysis treatment is specifically that 3% of the mass of the compound enzyme is added to the crushed forsythia, rhizoma coptidis, radix puerariae and gleditsiae sinensis seeds, and then enzymatic hydrolysis is performed at 45°C and pH 4.5 for 30 minutes, and then 80°C water bath inactivation is performed for 10 minutes.

3. The preparation method of the bubble bath liquid capable of clearing heat and reducing fire according to claim 2, wherein the low-temperature freeze-thaw activation treatment is specifically that the honeysuckle, honeysuckle flowers, mulberry leaves, andrographis leaves, mint, chrysanthemum and lophatheri leaves are first frozen at a temperature of-15°C for 2 hours, and then immediately sprayed with 30°C warm water for 3 minutes, and the process is repeated twice.

4. The preparation method of the bubble bath liquid capable of clearing heat and reducing fire according to claim 3, wherein the water extraction is specifically that 8 times the mass of water is added to the mixed activated raw materials, gleditsiae sinensis seed enzymatic hydrolysis powder and forsythia enzymatic hydrolysis powder, and then boiled for 10 minutes, and then the temperature is reduced to 50°C for 90 minutes of heat preservation extraction.

5. The preparation method of the bubble bath liquid capable of clearing heat and reducing fire according to claim 4, wherein the alcohol extraction is specifically that 6 times the mass of 50% ethanol is added to the mixed filter residue and radix puerariae enzymatic hydrolysis powder, and then cyclic reflux is performed at 60°C, and the process is repeated 3 times, and then vacuum extraction is performed to-0.06MPa for 5 minutes after each reflux.

6. The preparation method of the bubble bath liquid capable of clearing heat and reducing fire according to claim 5, wherein the low-temperature ultrasonic extraction is performed at a temperature of 25°C, an ultrasonic power of 200W, an ultrasonic mode of 3 seconds of work and 2 seconds of pause, and a total extraction time of 15 minutes.

7. The preparation method of the bubble bath liquid capable of clearing heat and reducing fire according to claim 6, wherein ​ ​ ​ ​ ​ The pulse stirring is specifically: stirring at 60 r / min for 30 seconds, pausing for 10 seconds, stirring at 120 r / min for 30 seconds, pausing for 10 seconds, repeating the step for 40 minutes.

8. The preparation method of the bubble bath liquid capable of clearing heat and reducing fire according to claim 7, characterized in that, The gradient concentration is specifically: first, the oil-in-water system is concentrated to 1 / 3 of the original volume at 45 DEG C under reduced pressure, and then the temperature is increased to 60 DEG C to continue the concentration to a relative density of 1.

08.

9. The preparation method of the bubble bath liquid capable of clearing heat and reducing fire according to claim 8, characterized in that, The sterilization treatment is specifically: first, microwave treatment at 300 W for 2 minutes, pausing for 10 seconds every 20 seconds during the treatment, and then ultraviolet irradiation at 254 nm for 20 minutes.

10. A bubble bath liquid capable of clearing heat and reducing fire, characterized in that, The bubble bath liquid capable of clearing heat and reducing fire prepared by the preparation method of any one of claims 1-9.

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