Double-liquid fractional extraction jingu shuchu hot compress liquid and preparation process thereof

Abstract

The present application relates to the technical field of herbal external preparation, in particular to a two-liquid fractional extraction Jingu Shuchu hot compress solution and a preparation process thereof, the present application splits the medicinal liquid into two sets of formula systems of a main soaking liquid large formula and a penetration-promoting soaking liquid small molecule, and adopts 55% ethanol and 75% ethanol aqueous solution fractional extraction respectively, the main soaking liquid is soaked for a long time with low alcohol by rhizome insect herb such as Corydalis, Chuanxiong, Rhabdophis, and Sinosenecio, for long-acting and relieving; the penetration-promoting soaking liquid is extracted for a short time with high alcohol by high-fat medicinal materials such as Frankincense, Myrrh, Dragon's Blood, and Wintergreen essential oil, to retain small-molecule penetration-promoting active ingredients. The present application solves the problems of uneven analysis of effective components in traditional herbal hot compress solution mixed soaking extraction, large loss of volatile components, low extraction rate of fat-soluble components, and many impurities easily irritating the skin, can improve the transdermal absorption capacity of the medicinal liquid, gently relieve the muscle soreness and discomfort of the neck, shoulder, waist, and leg, the extraction process is scientific, the finished product has strong stability, and the external use comfort is high.

Description

Technical Field

[0001] This invention relates to the field of herbal external preparations technology, and more specifically, to a two-liquid graded extraction muscle and bone soothing hot compress liquid and its preparation process. Background Technology

[0002] Neck, shoulder, lower back, and leg pain, muscle stiffness, and joint discomfort are common symptoms among those who work at desks, do manual labor, and the elderly. Currently, most herbal soothing hot compress solutions on the market use a single-proof alcohol mixture for extraction, which has several drawbacks. 1. When root, stem, insect and aromatic resin medicinal materials are mixed and soaked, a large amount of water-soluble macromolecular impurities, tannins and colloids are simultaneously precipitated, resulting in a product with many impurities. After application, it is easy to cause skin redness, stinging, itching and irritation. 2. Volatile penetration-enhancing ingredients such as borneol, camphor, and wintergreen essential oil are easily lost due to prolonged soaking in alcohol, resulting in a weak warm compress sensation, slow onset of action, and short duration of effect in the finished product. 3. In low-concentration alcohol, the effective components of fat-soluble blood-activating herbs such as frankincense, myrrh, and dragon's blood are insufficiently extracted, resulting in a weaker soothing effect. 4. The formula uses a crude extraction method, resulting in the simultaneous release of various medicinal components, an unbalanced combination of medicinal effects, poor transdermal absorption, and limited external soothing effects.

[0003] Therefore, existing hot compress solutions suffer from problems such as uneven precipitation, significant loss of volatile components, insufficient extraction of fat-soluble components, numerous impurities, weak soothing power, and easy skin irritation. There is an urgent need to develop a muscle and bone soothing hot compress solution with a reasonable extraction process, fewer impurities, low irritation, good transdermal effect, and long-lasting soothing effect. Summary of the Invention

[0004] In view of this, the present invention addresses the shortcomings of the prior art by proposing a two-liquid graded extraction muscle and bone soothing hot compress liquid and its preparation process, aiming to solve at least one of the problems mentioned in the background art.

[0005] On the one hand, the present invention provides a dual-liquid graded extraction muscle and bone soothing hot compress liquid, comprising: a compound of two herbal compositions consisting of a main extract (large formula) and a penetration-enhancing extract (small molecules); The main extract formula is composed of the following ingredients by weight: Corydalis rhizome or extract 26-32 parts, Ligusticum chuanxiong rhizome or extract 18-22 parts, Paeonia lactiflora rhizome or extract 13-17 parts, Paederia scandens vine or extract 10-14 parts, Spatholobus suberectus vine 10-14 parts, Dipsacus asper or extract 10-14 parts, Angelica pubescens rhizome or extract 13-17 parts, Notopterygium incisum rhizome or extract 13-17 parts, Achyranthes bidentata rhizome or extract 9-11 parts, Buthus martensii rhizome or extract 9-11 parts, Asarum heterotropoides rhizome or extract 9-11 parts, Ephedra sinica rhizome or extract 7-9 parts, Cinnamomum cassia twig or extract 7-9 parts, Carthamus tinctorius rhizome or extract 7-9 parts, Atractylodes macrocephala rhizome or extract 10 parts. ~14 parts, Zaocys dhumnades or extract 18-22 parts, Lycopodium clavatum or extract 18-22 parts, Drynaria fortunei or extract 10-14 parts, Eucommia ulmoides or extract 7-9 parts, Clematis chinensis or extract 13-17 parts, Angelica dahurica or extract 13-17 parts, Trachelospermum jasminoides or extract 7-9 parts, Zingiber officinale or extract 9-11 parts, Gentiana macrophylla 9-11 parts, Clematis armandii or extract 13-17 parts, Saposhnikovia divaricata or extract 13-17 parts, Panax notoginseng or extract 9-11 parts, Phellodendron chinense or extract 7-9 parts, Camphor or extract 4-6 parts, Borneol or extract 4-6 parts, Glycyrrhiza uralensis or extract 4-6 parts; The permeation-enhancing extract is composed of the following raw materials by weight: 18-22 parts of chili pepper or extract, 18-22 parts of pine needle or extract, 18-22 parts of dried tangerine peel or extract, 9-11 parts of safflower or extract, 9-11 parts of frankincense or extract, 9-11 parts of myrrh or extract, 9-11 parts of Bidens pilosa or extract, 18-22 parts of dragon's blood or extract, and 22-26 parts of wintergreen essential oil.

[0006] In some embodiments, the main extract is obtained by soaking and extracting with a 55% (v / v) aqueous ethanol solution; the permeation-enhancing extract is obtained by soaking and extracting with a 75% (v / v) aqueous ethanol solution.

[0007] On the other hand, the present invention provides a preparation process for a two-liquid graded extraction muscle and bone soothing hot compress liquid, comprising the following steps: S1. Raw material pretreatment: The herbal raw materials of each group of main extract and permeation-promoting extract are sorted, impurities are removed, washed and drained, and then crushed through a 20-40 mesh sieve. S2. Preparation of main extract by fractional extraction: Put the main extract raw material into the extraction tank, add 55% ethanol aqueous solution, seal and extract at room temperature for 30 days, and collect the extract by percolation in stages. S3. Preparation of permeation-enhancing extract: Put the permeation-enhancing extract raw material into another extraction tank, add 75% ethanol aqueous solution, seal and extract at room temperature for 15 days, and filter to obtain permeation-enhancing stock solution. S4. Compounding and blending: Mix the main leaching solution and the penetration-promoting leaching solution according to the set ratio, and add auxiliary materials for homogenization and blending. S5. After standing and maturing, precision filtration, and sterilization and filling, the finished muscle and bone soothing hot compress liquid is obtained.

[0008] In some embodiments, the extraction time of the main extract in step S2 is 30 days at room temperature; the extraction time of the permeation-promoting extract in step S3 is 15 days at room temperature.

[0009] In some embodiments, the volume ratio of the main immersion solution to the penetration-enhancing immersion solution is 9.5:1.5 to 8.5:1.0.

[0010] In some embodiments, the hot compress liquid is used in the preparation of external hot compress preparations for relieving soreness and swelling of neck, shoulder, waist and leg muscles and protecting tendons and bones.

[0011] Compared with existing technologies, the beneficial effects of this invention are as follows: The formula is divided into two systems: a main extract formula and a penetration-enhancing extract formula. Two different concentrations of ethanol solutions are used for stepwise extraction. Low-ethanol, prolonged soaking of root, stem, insect, and herbal ingredients extracts long-lasting, meridian-clearing components, while high-ethanol, short-time extraction of aromatic lipid-containing medicinal materials preserves small-molecule active substances. This increases the extraction rate of effective components, reduces the dissolution of irritating impurities, enhances transdermal absorption, and provides long-lasting relief for neck, shoulder, waist, and leg muscle soreness, fascia stiffness, and musculoskeletal strain discomfort. The above general description and the following detailed description are exemplary and explanatory only, and are not intended to limit this disclosure.

[0012] Other features and aspects of this disclosure will become clearer from the following detailed description of exemplary embodiments with reference to the accompanying drawings. Attached Figure Description

[0013] To more clearly illustrate the specific embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the specific embodiments or the prior art will be briefly introduced below. Obviously, the drawings described below are some embodiments of the present invention. For those skilled in the art, other drawings can be obtained from these drawings without creative effort.

[0014] Figure 1 The flowchart illustrates the preparation process of the two-liquid graded extraction muscle and bone soothing hot compress solution provided in this embodiment of the invention. Detailed Implementation

[0015] The technical solutions of the embodiments of this application will be clearly and completely described below with reference to the accompanying drawings. Obviously, the described embodiments are only some embodiments of this application, and not all embodiments. Based on the embodiments of this application, all other embodiments obtained by those of ordinary skill in the art without creative effort are within the scope of protection of this application.

[0016] See Figure 1As shown in the first embodiment, a two-liquid graded extraction muscle and bone soothing hot compress liquid according to the present application embodiment is prepared by compounding two groups of herbal compositions: a main extract of large-molecule ingredients and a penetration-promoting extract of small molecules. The main extract formula is composed of the following ingredients by weight: Corydalis rhizome or extract 26-32 parts, Ligusticum chuanxiong rhizome or extract 18-22 parts, Paeonia lactiflora rhizome or extract 13-17 parts, Paederia scandens vine or extract 10-14 parts, Spatholobus suberectus vine 10-14 parts, Dipsacus asper or extract 10-14 parts, Angelica pubescens rhizome or extract 13-17 parts, Notopterygium incisum rhizome or extract 13-17 parts, Achyranthes bidentata rhizome or extract 9-11 parts, Buthus martensii rhizome or extract 9-11 parts, Asarum heterotropoides rhizome or extract 9-11 parts, Ephedra sinica rhizome or extract 7-9 parts, Cinnamomum cassia twig or extract 7-9 parts, Carthamus tinctorius rhizome or extract 7-9 parts, Atractylodes macrocephala rhizome or extract 10 parts. ~14 parts, Zaocys dhumnades or extract 18-22 parts, Lycopodium clavatum or extract 18-22 parts, Drynaria fortunei or extract 10-14 parts, Eucommia ulmoides or extract 7-9 parts, Clematis chinensis or extract 13-17 parts, Angelica dahurica or extract 13-17 parts, Trachelospermum jasminoides or extract 7-9 parts, Zingiber officinale or extract 9-11 parts, Gentiana macrophylla 9-11 parts, Clematis armandii or extract 13-17 parts, Saposhnikovia divaricata or extract 13-17 parts, Panax notoginseng or extract 9-11 parts, Phellodendron chinense or extract 7-9 parts, Camphor or extract 4-6 parts, Borneol or extract 4-6 parts, Glycyrrhiza uralensis or extract 4-6 parts; The permeation-enhancing extract is composed of the following raw materials by weight: 18-22 parts of chili pepper or extract, 18-22 parts of pine needle or extract, 18-22 parts of dried tangerine peel or extract, 9-11 parts of safflower or extract, 9-11 parts of frankincense or extract, 9-11 parts of myrrh or extract, 9-11 parts of Bidens pilosa or extract, 18-22 parts of dragon's blood or extract, and 22-26 parts of wintergreen essential oil.

[0017] In some specific embodiments, the main extract is extracted by soaking in a 55% (v / v) aqueous ethanol solution; the permeation-enhancing extract is extracted by soaking in a 75% (v / v) aqueous ethanol solution.

[0018] The second embodiment, according to an embodiment of this application, includes the following steps in the preparation process of a two-liquid graded extraction muscle and bone soothing hot compress liquid: S1. Raw material pretreatment: The herbal raw materials of each group of main extract and permeation-promoting extract are sorted, impurities are removed, washed and drained, and then crushed through a 20-40 mesh sieve. S2. Preparation of main extract by fractional extraction: Put the main extract raw material into the extraction tank, add 55% ethanol aqueous solution, seal and extract at room temperature for 30 days, and collect the extract by percolation in stages. S3. Preparation of permeation-enhancing extract: Put the permeation-enhancing extract raw material into another extraction tank, add 75% ethanol aqueous solution, seal and extract at room temperature for 15 days, and filter to obtain permeation-enhancing stock solution. S4. Compounding and blending: Mix the main leaching solution and the penetration-promoting leaching solution according to the set ratio, and add auxiliary materials for homogenization and blending. S5. After standing and maturing, precision filtration, and sterilization and filling, the finished muscle and bone soothing hot compress liquid is obtained.

[0019] In some specific embodiments, the extraction time of the main extract in step S2 is 30 days at room temperature; the extraction time of the permeation-promoting extract in step S3 is 15 days at room temperature.

[0020] In some specific embodiments, the volume ratio of the main immersion solution to the permeation-enhancing immersion solution is 9.5:1.5 to 8.5:1.0.

[0021] In some specific embodiments, the hot compress liquid is used in the preparation of external hot compress preparations for relieving soreness and swelling of neck, shoulder, waist and leg muscles and protecting tendons and bones.

[0022] A two-liquid graded extraction muscle and bone soothing hot compress liquid, the raw materials are as follows by weight: Main extract formula: Corydalis rhizome 29 parts, Ligusticum chuanxiong rhizome 20 parts, Paeonia lactiflora rhizome 15 parts, Dipsacus asper rhizome 12 parts, Angelica pubescens rhizome 15 parts, Notopterygium incisum rhizome 15 parts, Achyranthes bidentata rhizome 10 parts, Buthus martensii rhizome 10 parts, Asarum sieboldii rhizome 10 parts, Ephedra sinica rhizome 8 parts, Cinnamomum cassia twig 8 parts, Carthamus tinctorius rhizome 8 parts, Atractylodes macrocephala rhizome 12 parts, Zaocys dhumnades 20 parts, Lycopodium clavatum rhizome 20 parts, Drynaria fortunei rhizome 12 parts, Spatholobus suberectus rhizome 10 parts, Paederia scandens rhizome 10 parts, Angelica dahurica rhizome 17 parts, Eucommia ulmoides rhizome 8 parts, Clematis chinensis rhizome 15 parts, Trachelospermum jasminoides rhizome 8 parts, Gentiana macrophylla rhizome 10 parts, Zingiber officinale rhizome 10 parts, Clematis chinensis rhizome 15 parts, Saposhnikovia divaricata rhizome 15 parts, Panax notoginseng rhizome 10 parts, Phellodendron chinense rhizome 8 parts, Camphor 5 parts, Borneol 5 parts, Glycyrrhiza uralensis rhizome 5 parts; Small molecules in the permeation-enhancing leachate: 20 parts chili pepper, 20 parts pine needle, 20 parts dried tangerine peel, 10 parts safflower, 10 parts frankincense, 10 parts myrrh, 20 parts dragon's blood, 10 parts Bidens pilosa, and 24 parts wintergreen essential oil.

[0023] Preparation process: 1. All raw materials are sorted, washed, drained, and pulverized through a 30-mesh sieve; 2. Add 55% ethanol to the main extract raw material, extract at 50℃ for 66 hours, and collect the extract by percolation; 3. Add 75% ethanol to the raw material for the penetration-enhancing extract, extract at 35°C for 30 hours, and filter to obtain the original penetration-enhancing extract; 4. The main immersion solution and the penetration-promoting immersion solution are mixed at a volume ratio of 8:2.

[0024] 5. Adjust the pH to 5.5, age in the dark for 6 days, filter and sterilize before filling to obtain the finished hot compress solution.

[0025] The muscle and bone soothing hot compress solution prepared by this invention can be applied externally as a poultice or wet compress to the neck, shoulders, back, lumbar spine, and joints of the limbs to relieve muscle soreness, stiffness, and discomfort, thus providing a soothing and protective effect on muscles and bones. This product should be used with caution by pregnant women and children, and is contraindicated on broken skin. It should not be allowed to enter the mouth or nasal cavity or its mucous membranes. Store at room temperature, away from light and in a well-ventilated area.

[0026] This embodiment provides a two-liquid graded extraction muscle and bone soothing hot compress liquid, which is prepared by compounding two groups of herbal compositions, namely the main extract and the penetration-promoting extract, in a volume ratio of 9:1.

[0027] The main extract formula is composed of the following ingredients by weight: Corydalis rhizome 29 parts, Ligusticum chuanxiong rhizome 20 parts, Paeonia lactiflora rhizome 15 parts, Paederia scandens vine 12 parts, Spatholobus suberectus vine 12 parts, Dipsacus asper 12 parts, Angelica pubescens rhizome 15 parts, Notopterygium incisum rhizome 15 parts, Achyranthes bidentata rhizome 10 parts, Buthus martensii rhizome 10 parts, Asarum sieboldii rhizome 10 parts, Ephedra sinica rhizome 8 parts, Cinnamomum cassia twig 8 parts, Carthamus tinctorius rhizome 8 parts, Atractylodes macrocephala rhizome 12 parts, Zaocys dhumnades 20 parts, Lycopodium clavatum rhizome 20 parts, Drynaria fortunei rhizome 12 parts, Eucommia ulmoides rhizome 8 parts, Clematis chinensis rhizome 15 parts, Angelica dahurica rhizome 15 parts, Trachelospermum jasminoides rhizome 8 parts, Zingiber officinale rhizome 10 parts, Gentiana macrophylla rhizome 10 parts, Clematis chinensis rhizome 15 parts, Saposhnikovia divaricata rhizome 15 parts, Panax notoginseng rhizome 10 parts, Phellodendron chinense rhizome 8 parts, Camphor 5 parts, Borneol 5 parts, Glycyrrhiza uralensis rhizome 5 parts.

[0028] The permeation-enhancing extract is composed of the following raw materials by weight: 20 parts chili pepper, 20 parts pine needle, 20 parts dried tangerine peel, 10 parts safflower, 10 parts frankincense, 10 parts myrrh, 10 parts Bidens pilosa, 20 parts dragon's blood, and 24 parts wintergreen essential oil.

[0029] Its preparation process includes the following steps: S1. Raw material pretreatment: The herbal raw materials of each group of main extract and penetration-promoting extract are sorted and impurities are removed, rinsed with clean water and drained, placed in a ventilated and cool place to dry the surface moisture, and then put into a pulverizer to grind them, pass through a 30-mesh sieve, and set aside for later use. S2. Preparation of main extract by fractional extraction: The main extract raw material is put into a percolation tank, and 8 times the volume of 55% ethanol aqueous solution is added. After stirring evenly, the tank is sealed and soaked at room temperature of 20±5℃ for 48 hours to allow the medicinal material to fully swell. Then, the percolation is started, and the percolation rate is controlled to be 2-3 ml per kilogram of medicinal material per minute. The percolation liquid is collected in several batches. During the percolation process, 55% ethanol aqueous solution is continuously added until the percolation liquid reaches 6 times the total weight of the raw material. The percolation is then stopped, and the main extract raw materials collected from each batch are combined for later use. S3. Preparation of the enhanced penetration extract: The enhanced penetration extract raw materials (excluding wintergreen essential oil) are put into another extraction tank, and 6 times the total weight of the raw materials are added to a 75% ethanol aqueous solution. After stirring evenly, the tank is sealed and extracted at room temperature of 20±5℃ for 15 days, stirring once every 2 days for 30 minutes each time. After extraction, the solution is filtered through a 200-mesh filter cloth and the filtrate is collected. Wintergreen essential oil is added to the filtrate and stirred evenly to obtain the enhanced penetration stock solution for later use. S4. Compounding and Blending: Pump the main extract stock solution and the penetration-enhancing extract solution into the blending tank at a volume ratio of 9:1, start stirring, and control the speed at 60 r / min; add the excipients in sequence: 3 parts glycerol, 2 parts propylene glycol, 1.5 parts Tween-80, and 0.2 parts vitamin E, and continue stirring for 30 min until the system is homogeneous; then use a high-speed homogenizer to homogenize at 8000 r / min for 5 min to obtain a homogenized drug solution; S5. Static Aging and Filtration Sterilization: Add 0.1 mol / L citric acid solution to the homogenized medicinal solution to adjust the pH value to 5.5±0.3; transfer the medicinal solution to a sealed storage tank and let it stand for 7 days under light-proof and room temperature conditions to allow the medicinal solution to fully age and impurities to settle naturally; after aging, first filter it through a 0.45μm microporous membrane, then filter it aseptically through a 0.22μm polyvinylidene fluoride (PVDF) membrane, and finally fill and seal it in a Class 100 clean environment to obtain the finished muscle and bone soothing hot compress solution.

[0030] This embodiment uses a high compound ratio of 9:1 between the main extract and the penetration-enhancing extract. The main extract has a large proportion and a high content of long-acting, meridian-clearing and soothing ingredients, making it suitable for deep soothing and conditioning of chronic musculoskeletal strain and muscle stiffness. The 55% low-alcohol room-temperature percolation process allows the large molecular active ingredients such as alkaloids, flavonoids, and saponins in root, stem, and insect medicinal materials to dissolve slowly and fully, while reducing the precipitation of irritating impurities such as tannins, gums, and proteins. The 75% high-alcohol short-time extraction process retains the fat-soluble resin acid components in frankincense, myrrh, and dragon's blood, as well as volatile penetration-enhancing components such as methyl salicylate in wintergreen essential oil to the greatest extent, avoiding the loss of volatile components caused by long-term soaking. Example

[0031] This embodiment provides a two-liquid graded extraction muscle and bone soothing hot compress liquid. Its raw material composition and preparation process are basically the same as those in Embodiment 1, except that the volume ratio of the main extract to the penetration-enhancing extract is 8.8:1.2.

[0032] In this embodiment, the ratio of main soaking solution to penetration enhancer solution is moderate, balancing long-lasting soothing with rapid onset of action. The content of transdermal penetration enhancer ingredients is moderate, and the warming sensation is gentle and long-lasting, making it suitable for daily neck, shoulder, waist and leg soothing care for most people. Example

[0033] This embodiment provides a two-liquid graded extraction muscle and bone soothing hot compress liquid. Its raw material composition and preparation process are basically the same as those in Embodiment 1, except that the volume ratio of the main extract to the penetration-enhancing extract is 8.5:1.5.

[0034] This embodiment has a higher proportion of penetration-enhancing extract, and a higher content of transdermal penetration-enhancing and warming components, resulting in a faster onset of action and a noticeable warming sensation. It is suitable for rapid relief of acute muscle soreness and joint discomfort. The increased content of penetration-enhancing components can accelerate the transdermal absorption of the active ingredients in the main extract and shorten the onset of action. However, attention should be paid to skin tolerance during use. It is recommended that sensitive skin start with a low concentration.

[0035] Example 4 (Extract Substitution Implementation) This embodiment provides a two-liquid graded extraction muscle and bone soothing hot compress liquid, whose raw material composition and preparation process are basically the same as those in Embodiment 1, the only difference being that: the Corydalis rhizome in the main extract is replaced by Corydalis rhizome extract, and the Ligusticum chuanxiong rhizome is replaced by Ligusticum chuanxiong extract.

[0036] The preparation method of the Corydalis extract is as follows: take Corydalis slices, add 10 times the volume of 60% ethanol aqueous solution, heat and reflux to extract twice, 1.5h each time, combine the extracts, filter, recover ethanol from the filtrate under reduced pressure and concentrate to a clear extract with a relative density of 1.10-1.15 (measured at 60℃), spray dry, and pulverize into fine powder to obtain the Corydalis extract, wherein the content of corydaline is not less than 0.5%.

[0037] The preparation method of the Ligusticum chuanxiong extract is as follows: take Ligusticum chuanxiong slices, add 8 times the volume of 70% ethanol aqueous solution, heat and reflux to extract twice, 1 hour each time, combine the extracts, filter, recover the ethanol from the filtrate under reduced pressure and concentrate to a clear extract with a relative density of 1.08-1.12 (measured at 60℃), spray dry, and pulverize into fine powder to obtain the Ligusticum chuanxiong extract, wherein the ferulic acid content is not less than 0.2%.

[0038] In this embodiment, some medicinal extracts are used to replace the original medicinal materials, which can reduce the extraction time and improve production efficiency. At the same time, the content of effective components in the extract is more stable, and the quality of the finished product is more uniform. The use of extracts is equivalent to pre-purifying the raw materials, which can further reduce the impurity content in the medicinal solution and reduce skin irritation.

[0039] Supplementary Comparison Comparative Example 1 (Traditional single ethanol mixing process) This comparative example uses a traditional herbal hot compress preparation process, in which all medicinal materials are mixed and then extracted by soaking in a single concentration of ethanol.

[0040] The ingredients, by weight, are: Corydalis Rhizome 29 parts, Ligusticum Rhizome 20 parts, White Peony Root 15 parts, Paederia Sinensis Vine 12 parts, Spatholobus Stem 12 parts, Dipsacus Root 12 parts, Angelica Pubescens Root 15 parts, Notopterygium Root 15 parts, Achyranthes Root 10 parts, Scorpion 10 parts, Asarum 10 parts, Ephedra Root 8 parts, Cinnamon Twig 8 parts, Safflower 18 parts, Atractylodes Rhizome 12 parts, Zaocys Sinensis Root 20 parts, Lycopodium Root 20 parts, Drynaria Rhizome 12 parts, Eucommia Bark 8 parts, Clematis chinensis 15 parts, Angelica dahurica 15 parts, Trachelospermum jasminoides 8 parts, dried ginger 10 parts, Gentiana macrophylla 10 parts, Clematis armandii 15 parts, Saposhnikovia divaricata 15 parts, Panax notoginseng 10 parts, Phellodendron chinense 8 parts, camphor 5 parts, borneol 5 parts, licorice 5 parts, chili pepper 20 parts, pine needle 20 parts, dried tangerine peel 20 parts, frankincense 10 parts, myrrh 10 parts, Bidens pilosa 10 parts, dragon's blood 20 parts, wintergreen essential oil 24 parts.

[0041] Preparation process: All raw materials are sorted, cleaned and drained, crushed and passed through a 30-mesh sieve, and put into the same extraction tank. Add 8 times the total weight of the raw materials in a 65% ethanol aqueous solution. Seal and extract at room temperature for 30 days. Filter and collect the extract. Add 3 parts glycerol, 2 parts propylene glycol and 1.5 parts Tween-80, and stir evenly. Adjust the pH to 5.5, let stand and mature for 7 days, filter and fill into the container to obtain the control hot compress solution.

[0042] Supplemental effect verification test The hot compress solutions prepared in Examples 1, 3, and Comparative Example 1 were used respectively, and the contents of three representative active ingredients—tetrahydropalmatine, ferulic acid, and methyl salicylate—were determined by high-performance liquid chromatography (HPLC). The chromatographic conditions were as follows: for tetrahydropalmatine, a C18 column was used with a mobile phase of methanol-0.1% phosphoric acid solution (55:45) and a detection wavelength of 280 nm; for ferulic acid, a C18 column was used with a mobile phase of acetonitrile-0.1% phosphoric acid solution (18:82) and a detection wavelength of 316 nm; for methyl salicylate, a C18 column was used with a mobile phase of methanol-water (60:40) and a detection wavelength of 305 nm.

[0043] The test results showed that in Example 1, the content of fumaric acid was 42.6 μg / ml, the content of ferulic acid was 28.9 μg / ml, and the content of methyl salicylate was 186.3 μg / ml; in Example 3, the content of fumaric acid was 40.3 μg / ml, the content of ferulic acid was 27.5 μg / ml, and the content of methyl salicylate was 215.7 μg / ml; and in Comparative Example 1, the content of fumaric acid was 31.8 μg / ml, the content of ferulic acid was 22.1 μg / ml, and the content of methyl salicylate was 98.5 μg / ml.

[0044] As can be seen from the above results, compared with Comparative Example 1 using the traditional mixed-soaking process, the hot compress solution prepared in this embodiment of the invention shows an increase of approximately 34% in corydaline, approximately 31% in ferulic acid, and approximately 89%–119% in methyl salicylate. Among these, methyl salicylate, as the main active ingredient of wintergreen essential oil, shows the most significant increase in content, indicating that the graded extraction process of this invention, especially the use of 75% high-alcohol short-time extraction for the permeation-promoting extract, effectively reduces the loss of volatile components and significantly improves the retention rate of both fat-soluble and volatile active ingredients. The use of 55% low-alcohol percolation process for the main extract also allows for more complete extraction of alkaloids and phenolic acids from rhizomes.

[0045] Experimental Example 2: In vitro transdermal absorption test In vitro transdermal absorption assays were conducted using a modified Franz diffusion cell. Abdominal skin was harvested from healthy male SD rats, subcutaneous adipose tissue was removed, and the skin was rinsed thoroughly with physiological saline. The skin was then fixed between the supply and receiving cells of the diffusion cell, with the stratum corneum facing the supply cell. The receiving cell contained 6.5 ml of pH 7.4 phosphate-buffered saline as the receiving solution, maintained at 32°C, and stirred at 300 rpm. 1 ml each of the hot compress solutions from Example 1 and Comparative Example 1 were added to the supply cell. Samples of 0.5 ml were taken at 1, 2, 4, 6, 8, and 12 hours, and an equal volume of isothermal receiving solution was added simultaneously. The content of corydaline in the receiving solution was determined by HPLC, and the cumulative permeation per unit area was calculated.

[0046] The experimental results showed that the cumulative permeation of corydaline in Example 1 over 1 hour was 2.15 ± 0.32 μg / cm³. 2 The concentration at 2 hours was 4.68 ± 0.59 μg / cm³. 2 The concentration at 4 hours was 9.82 ± 1.05 μg / cm³. 2 The concentration at 6 hours was 15.34 ± 1.68 μg / cm³. 2 The concentration at 8 hours was 21.56 ± 2.13 μg / cm³. 2 The concentration at 12h was 32.48 ± 3.25 μg / cm³. 2 The cumulative permeation of corydaline in Comparative Example 1 over 1 hour was 0.87 ± 0.18 μg / cm³. 2 The concentration at 2h was 2.03 ± 0.35 μg / cm³. 2 The concentration at 4h was 4.56 ± 0.72 μg / cm³. 2 The concentration at 6 hours was 7.23 ± 1.04 μg / cm³. 2 The concentration at 8 hours was 10.15 ± 1.37 μg / cm³. 2 The concentration at 12h was 15.62 ± 1.98 μg / cm³. 2 .

[0047] As can be seen from the above results, the cumulative permeation of corydalis ethylsaturate in the hot compress solution of Example 1 of the present invention was significantly higher than that of Comparative Example 1 at all time points, and the cumulative permeation at 12 hours was approximately 2.08 times that of Comparative Example 1. Meanwhile, Example 1 showed significant transdermal absorption at 1 hour, indicating a faster onset of action. This demonstrates that the permeation-enhancing components in the permeation-enhancing extract, such as capsaicin, wintergreen essential oil, and frankincense and myrrh resin, effectively opened the channels of the stratum corneum of the skin, promoting the transdermal absorption of the active ingredients in the main extract. This proves that the dual-liquid graded extraction and main-enhancing-enhancing process design of the present invention can significantly improve the transdermal absorption efficiency of the medicinal solution and enhance the external soothing effect.

[0048] Test Example 3: Skin Irritation Test The skin irritation / corrosiveness test method was conducted according to the "Cosmetic Safety Technical Specifications" (2015 edition). Six healthy New Zealand white rabbits, half male and half female, were randomly divided into three groups of two rabbits each. Twenty-four hours before the test, the fur on both sides of the rabbit's spine was shaved, with each area approximately 3cm × 3cm. 0.5ml of the hot compress solution from Examples 1, 3, and Comparative Example 1 was applied to the left side of the shaved skin, while physiological saline was applied to the right side as a control. After application, the skin was covered with two layers of gauze and one layer of cellophane, and secured with adhesive tape. The left side of each animal was treated with the test substance, while the right side served as a blank control. Four hours after application, the residual test substance was removed with warm water. Skin reactions at the application sites were observed at 1, 24, 48, and 72 hours after removal. Erythema and edema were scored according to the scoring criteria, and the average score at each time point was calculated.

[0049] The experimental results showed that the average scores at each time point in Example 1 were 0.33 at 1 hour, 0.17 at 24 hours, 0 at 48 hours, and 0 at 72 hours, with the highest average score being 0.33, indicating no irritation. The average scores at each time point in Example 3 were 0.67 at 1 hour, 0.33 at 24 hours, 0.17 at 48 hours, and 0 at 72 hours, with the highest average score being 0.67, indicating no irritation. The average scores at each time point in Comparative Example 1 were 1.50 at 1 hour, 1.17 at 24 hours, 0.67 at 48 hours, and 0.33 at 72 hours, with the highest average score being 1.50, indicating mild irritation.

[0050] As can be seen from the above results, the hot compress solutions of Examples 1 and 3 of the present invention are not irritating to rabbit skin, and the highest average score is far below the mild irritation evaluation standard; while the comparative example 1 of the traditional process showed mild irritation. The results indicate that the two-liquid graded extraction process of the present invention, through the graded extraction method of low-alcohol long-soaking main extract and high-alcohol short-time penetration-enhancing extract, reduces the dissolution of large molecular irritating impurities such as tannins, colloids, and proteins, while avoiding irritating byproducts generated by long-term soaking of volatile components, significantly reducing the skin irritation of the hot compress solution and improving the external application safety and user comfort.

[0051] Stability Study in Experiment Example 4 The hot compress solution prepared in Example 1 was placed in a constant temperature and humidity chamber and accelerated stability test was carried out under the conditions of 40℃±2℃ and 75%±5% relative humidity. Samples were taken at 0, 1, 2 and 3 months to examine the properties, pH value, visible foreign matter, content of effective ingredients and other indicators.

[0052] The results showed that at 0 months, the sample was a clear, brownish-red liquid with a pH of 5.48. Visible foreign matter was within the acceptable range, with fumaric acid content of 42.6 μg / ml and methyl salicylate content of 186.3 μg / ml. At 1 month, the sample was still a clear, brownish-red liquid with a pH of 5.45. Visible foreign matter was within the acceptable range, with fumaric acid content of 42.1 μg / ml and methyl salicylate content of 182.5 μg / ml. At 2 months, the sample was a clear, brownish-red liquid with a pH of 5.42. Visible foreign matter was within the acceptable range, with fumaric acid content of 41.5 μg / ml and methyl salicylate content of 178.6 μg / ml. At 3 months, the sample was a clear, brownish-red liquid without precipitation, with a pH of 5.38. Visible foreign matter was within the acceptable range, with fumaric acid content of 40.8 μg / ml and methyl salicylate content of 174.2 μg / ml.

[0053] As can be seen from the above results, after 3 months of accelerated testing, the properties, pH value, and visible foreign matter of the hot compress solution of this invention showed no significant changes. The retention rates of corydaline and methyl salicylate were 95.8% and 93.5%, respectively, both within the acceptable range. This indicates that the graded extraction process and formulation design of this invention are reasonable, the finished product has good stability, and its quality is controllable within the shelf life.

[0054] Obviously, those skilled in the art can make various modifications and variations to this invention without departing from its spirit and scope. Therefore, if these modifications and variations fall within the scope of the claims of this invention and their equivalents, this invention also intends to include these modifications and variations.

Claims

1. A two-liquid graded extraction muscle and bone soothing hot compress liquid, characterized in that: It is prepared by combining two herbal compositions: a main extract (large formula) and a penetration-enhancing extract (small molecules). The main extract formula is composed of the following ingredients by weight: Corydalis rhizome or extract 26-32 parts, Ligusticum chuanxiong rhizome or extract 18-22 parts, Paeonia lactiflora rhizome or extract 13-17 parts, Paederia scandens vine or extract 10-14 parts, Spatholobus suberectus vine 10-14 parts, Dipsacus asper or extract 10-14 parts, Angelica pubescens rhizome or extract 13-17 parts, Notopterygium incisum rhizome or extract 13-17 parts, Achyranthes bidentata rhizome or extract 9-11 parts, Buthus martensii rhizome or extract 9-11 parts, Asarum heterotropoides rhizome or extract 9-11 parts, Ephedra sinica rhizome or extract 7-9 parts, Cinnamomum cassia twig or extract 7-9 parts, Carthamus tinctorius rhizome or extract 7-9 parts, Atractylodes macrocephala rhizome or extract 10 parts. ~14 parts, Zaocys dhumnades or extract 18-22 parts, Lycopodium clavatum or extract 18-22 parts, Drynaria fortunei or extract 10-14 parts, Eucommia ulmoides or extract 7-9 parts, Clematis chinensis or extract 13-17 parts, Angelica dahurica or extract 13-17 parts, Trachelospermum jasminoides or extract 7-9 parts, Zingiber officinale or extract 9-11 parts, Gentiana macrophylla 9-11 parts, Clematis armandii or extract 13-17 parts, Saposhnikovia divaricata or extract 13-17 parts, Panax notoginseng or extract 9-11 parts, Phellodendron chinense or extract 7-9 parts, Camphor or extract 4-6 parts, Borneol or extract 4-6 parts, Glycyrrhiza uralensis or extract 4-6 parts; The permeation-enhancing extract is composed of the following raw materials by weight: 18-22 parts of chili pepper or extract, 18-22 parts of pine needle or extract, 18-22 parts of dried tangerine peel or extract, 9-11 parts of safflower or extract, 9-11 parts of frankincense or extract, 9-11 parts of myrrh or extract, 9-11 parts of Bidens pilosa or extract, 18-22 parts of dragon's blood or extract, and 22-26 parts of wintergreen essential oil.

2. The dual-liquid graded extraction muscle and bone soothing hot compress liquid according to claim 1, characterized in that: The main extract is obtained by soaking and extracting with a 55% (v / v) ethanol aqueous solution; the permeation-enhancing extract is obtained by soaking and extracting with a 75% (v / v) ethanol aqueous solution.

3. A preparation process for the two-liquid graded extraction muscle-relaxing hot compress liquid according to any one of claims 1 to 2, characterized in that, Includes the following steps: S1. Raw material pretreatment: The herbal raw materials of each group of main extract and permeation-promoting extract are sorted, impurities are removed, washed and drained, and then crushed through a 20-40 mesh sieve. S2. Preparation of main extract by fractional extraction: Put the main extract raw material into the extraction tank, add 55% ethanol aqueous solution, seal and extract at room temperature for 30 days, and collect the extract by percolation in stages. S3. Preparation of permeation-enhancing extract: Put the permeation-enhancing extract raw material into another extraction tank, add 75% ethanol aqueous solution, seal and extract at room temperature for 15 days, and filter to obtain permeation-enhancing stock solution. S4. Compounding and blending: Mix the main leaching solution and the penetration-promoting leaching solution according to the set ratio, and add auxiliary materials for homogenization and blending. S5. After standing and maturing, precision filtration, and sterilization and filling, the finished muscle and bone soothing hot compress liquid is obtained.

4. The preparation process according to claim 2, characterized in that: In step S2, the main extract is extracted at room temperature for 30 days; in step S3, the permeation-promoting extract is extracted at room temperature for 15 days.

5. The preparation process according to claim 2, characterized in that: The volume ratio of the main leaching solution to the permeation-promoting leaching solution is 9.5:1.5 to 8.5:1.

0.

6. The application of the hot compress liquid according to claim 1 in the preparation of a topical hot compress preparation for relieving soreness and swelling of the neck, shoulders, waist and legs, and protecting muscles and bones.

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