CN116570690A - Herbal composition for acupoint plaster for improving sleep and acupoint plaster - Google Patents
Herbal composition for acupoint plaster for improving sleep and acupoint plaster Download PDFInfo
- Publication number
- CN116570690A CN116570690A CN202310555048.8A CN202310555048A CN116570690A CN 116570690 A CN116570690 A CN 116570690A CN 202310555048 A CN202310555048 A CN 202310555048A CN 116570690 A CN116570690 A CN 116570690A
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- extract
- herbal composition
- acupoint
- water
- microemulsion
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- A61K2236/30—Extraction of the material
- A61K2236/39—Complex extraction schemes, e.g. fractionation or repeated extraction steps
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/50—Methods involving additional extraction steps
- A61K2236/51—Concentration or drying of the extract, e.g. Lyophilisation, freeze-drying or spray-drying
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/50—Methods involving additional extraction steps
- A61K2236/53—Liquid-solid separation, e.g. centrifugation, sedimentation or crystallization
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/50—Methods involving additional extraction steps
- A61K2236/55—Liquid-liquid separation; Phase separation
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A50/00—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
- Y02A50/30—Against vector-borne diseases, e.g. mosquito-borne, fly-borne, tick-borne or waterborne diseases whose impact is exacerbated by climate change
Abstract
The invention discloses an acupoint plaster herbal composition for improving sleep and an acupoint plaster, which comprise the following raw materials: radix Stemonae, radix Sophorae Flavescentis, saviae Miltiorrhizae radix extract, rhizoma Ligustici Chuanxiong extract, natural Borneolum, chlorhexidine acetate, microemulsion, carbomer-940, and water. Compared with the prior art, the herbal composition for the acupoint plaster is matched with the acupoint plaster for use, is convenient to use, has quick and durable effect, can achieve the effects of warming channels and activating collaterals, relieving angina, relieving coronary heart disease, promoting sleep, refreshing brain and the like, has higher storage stability and transdermal efficiency, and does not damage skin structures and cause erythema.
Description
Technical Field
The invention relates to the technical field of medicine patches, in particular to an acupoint patch herbal composition for improving sleep and an acupoint patch.
Background
The acupoint plaster is a Chinese medicine external plaster, and can regulate physiological function of human body by means of permeation of medicine components in acupoint so as to attain the goal of curing diseases or improving health. The existing acupoint application technology mainly comprises the following traditional Chinese medicine acupoint application technology, electronic acupoint application technology, phototherapy acupoint application technology and microneedle acupoint application technology: the Chinese medicine acupoint plaster is acupoint plaster prepared with Chinese medicine plaster, and is suitable for treating various diseases. The Chinese medicinal acupoint plaster is prepared from Chinese medicinal materials by grinding, refining, and making into preparation, and has effects of warming and dredging channels and collaterals, removing blood stasis, relieving pain, clearing heat and detoxicating. The electronic acupoint plaster is a new type acupoint plaster technology, and can produce small current to stimulate acupoint by means of electronic chip adhered to acupoint so as to attain the goal of regulating physiological function of human body. The electronic acupoint plaster is suitable for treating insomnia, pain, anxiety, etc. Phototherapy acupoint plaster is an acupoint plaster technology which uses light energy to stimulate acupoints. The light energy is converted into biological energy through the photosensitive patch stuck on the acupoint to stimulate the acupoint so as to achieve the purpose of regulating the physiological function of human body. The phototherapy acupoint plaster is suitable for treating dermatoses, pain, etc. The micro-needle acupoint plaster is an acupoint plaster technology which uses micro-needles to stimulate acupoints. The micro-needle patch stuck on the acupoint stimulates the acupoint, promotes local blood circulation, relieves symptoms such as pain, spasm and inflammation, and achieves the aims of treatment and health care.
The following problems still exist in the traditional Chinese medicine acupoint pasting technology: the application position is not accurate enough, and the treatment effect of the acupoint application is affected. The permeation rate and permeation amount of the pharmaceutical ingredient are difficult to control, so that excessive or insufficient conditions may occur, which affect the therapeutic effect. The medicinal components in the Chinese medicinal acupoint plaster may cause uncomfortable reactions such as allergy and skin irritation, and the problems of infirm plaster, falling off and the like may occur in the plaster process, so that the treatment effect is affected, and the long-term storage functional molecules are easy to deteriorate and lose the curative effect.
Therefore, when preparing the acupoint plaster, attention is paid to defects and limitations of the acupoint plaster, and the design of functional substances is combined, so that the treatment effect is promoted, and the uncomfortable response is reduced.
The invention patent application CN115671170A discloses a composition for acupoint application for improving sleep disorder of children, acupoint application and application, and belongs to the field of traditional Chinese medicines. The composition comprises the following components in parts by weight: 5-15 parts of astragalus, 8-15 parts of codonopsis pilosula, 5-12 parts of bighead atractylodes rhizome, 8-12 parts of moutan bark and 5-10 parts of peppermint. The invention takes astragalus root, pilose asiabell root, largehead atractylodes rhizome, tree peony bark and peppermint as raw materials, is compatible to prepare a traditional Chinese medicine composition capable of improving the sleeping quality of children, combines the combined action of acupoints, and stimulates acupoints of Zusanli, shenque and Pi to invigorate the spleen and tranquilize the mind by the traditional Chinese medicine; liver acupoints, yongquan, clear internal heat; the interaction of the Shendao tranquillization and the acupuncture points of the whole body is stimulated to achieve the effects of strengthening spleen, clearing heat and tranquillization. The invention adopts the external treatment method of traditional Chinese medicine to treat the sleep disorder of children, promotes the deep sleep of children, combines the pure traditional Chinese medicine treatment with the dialectical selection of acupoints of traditional Chinese medicine, is safe, simple and convenient to operate, and has no toxic or side effect. However, the composition for acupoint application prepared by the invention has the problems of insufficient transdermal effect, poor storage stability and unsatisfactory effect of improving sleep disorder.
Disclosure of Invention
In view of the defects of insufficient transdermal effect, poor storage stability and unsatisfactory effect of improving sleep disorder of the herbal composition for acupoint application in the prior art, the invention aims to provide the herbal composition for acupoint application and the acupoint application for improving sleep.
In order to achieve the above object, the present invention adopts the following technical scheme:
an acupoint application herbal composition for improving sleep comprises the following raw materials: radix Stemonae, radix Sophorae Flavescentis, saviae Miltiorrhizae radix extract, rhizoma Ligustici Chuanxiong extract, natural Borneolum, chlorhexidine acetate, microemulsion, carbomer-940, and water.
Preferably, the herbal composition for acupoint application for improving sleep comprises the following raw materials in percentage by weight: 1 to 3 percent of radix stemonae, 1 to 3 percent of radix sophorae flavescentis, 2 to 5 percent of radix salviae miltiorrhizae extract, 2 to 5 percent of rhizoma ligustici wallichii extract, 1 to 2 percent of natural borneol, 0.01 to 0.3 percent of chlorhexidine acetate, 5 to 10 percent of microemulsion, 1 to 2 percent of carbomer-940 and 100 percent of water.
The preparation method of the herbal composition comprises the following steps:
step 1, weighing the raw materials according to the weight percentage, adding radix stemonae, radix sophorae flavescentis, radix salviae miltiorrhizae extract, ligusticum wallichii extract, natural borneol and chlorhexidine acetate into the microemulsion, then adding the mixture into water, and stirring at 100-500 rpm for 1-3 hours to obtain a functional agent;
and 2, adding carbomer-940 into water, standing overnight, adding 10-22 wt% potassium bicarbonate aqueous solution to adjust the pH to be neutral, adding the functional agent prepared in the step 1, and stirring at 100-500 rpm for 1-3 h to obtain the herbal composition.
The preparation method of the salvia miltiorrhiza extract comprises the following steps:
removing impurities from radix salviae miltiorrhizae, adding water with the mass of 8-12 times, heating and extracting for 0.5-3 h at 60-90 ℃, filtering by a sieve with 50-200 meshes, reserving filtrate, adding water with the mass of 4-8 times into dregs, heating and extracting for 1-3 times at 60-90 ℃, filtering by a sieve with 50-200 meshes each time, merging filtrate, concentrating under reduced pressure at 40-60 ℃ until the relative density is 1.03-1.06, concentrating under reduced pressure at the vacuum degree of 0.08-0.095 Mpa, and rotating at 30-100 rpm to obtain concentrated solution; cooling to room temperature, adding 80-95 wt% ethanol water solution with the mass of 0.8 times, standing for 5-24 h, filtering by a 100-300 mesh sieve, recovering ethanol to obtain crude drug, adsorbing by macroporous adsorption resin AB-8, wherein the mass ratio of the crude drug to the macroporous adsorption resin AB-8 is 1: 2-5, washing with water until effluent liquid has no sugar reaction, and continuing to use 20-50wt% ethanol water solution for elution until the eluent is added with ferric trichloride and potassium ferricyanide reagent to turn green and no precipitation; concentrating the eluent at 40-60 ℃ until the relative density is 1.25-1.3, and spray drying to obtain the salvia miltiorrhiza extract.
The preparation method of the ligusticum chuanxiong hort extract comprises the following steps:
reflux-extracting rhizoma Ligustici Chuanxiong with 3-7 times of 80-95wt% ethanol water solution at 60-80deg.C for 1-3 times, 50-100 min each time, mixing filtrates, concentrating under reduced pressure to obtain extract, concentrating under reduced pressure at vacuum degree of 0.08-0.095 Mpa and rotation speed of 30-100 rpm; adding the extract into water with the mass of 3-7 times, adsorbing by using macroporous adsorption resin AB-8, eluting by using 20-40 wt% ethanol water solution with the mass of 15-25 times of the extract, combining the eluates, removing ethanol under reduced pressure, drying in vacuum for 3-8 hours at the temperature of 30-50 ℃ to obtain the ligusticum chuanxiong hort extract.
The preparation method of the natural borneol comprises the following steps:
z1, cleaning and drying branches and leaves of borneol camphor trees, and then crushing the branches and leaves of borneol camphor trees and sieving the crushed branches and leaves of borneol camphor trees with a 30-100-mesh sieve to obtain borneol camphor branch and leaf powder; adding borneol camphor branch and leaf powder into an ethanol water solution with the mass of 20-40 wt% which is 5-10 times, carrying out ultrasonic treatment for 20-40 min at the temperature of 30-50 ℃ under the ultrasonic power of 400-600W, filtering with 50-200 meshes, collecting filtrate, carrying out ultrasonic extraction on residues for 1-3 times, merging the filtrate, carrying out reduced pressure distillation to form paste, carrying out reduced pressure concentration, wherein the vacuum degree is 0.08-0.095 Mpa, and the rotating speed is 30-100 rpm, thus obtaining crude natural borneol extract;
z2, the crude extract of the natural borneol prepared in the step Z1 is prepared according to the solid-liquid mass ratio of 1:1 to 3, adding tetrahydrofuran-n-octanol-water, then swirling for 10 to 30 seconds, centrifuging for 3 to 8 minutes at 10000 to 20000rpm, wherein the mass ratio of the tetrahydrofuran, the n-octanol and the water is 0.8 to 1.2: 1-2: 1.5 to 2.5, and after the supernatant is poured off, the solid-liquid mass ratio is 1: adding petroleum ether into 2-4 parts, putting into a water bath kettle, stirring and heating at 100-500 rpm, heating at 40-60 ℃ until the petroleum ether is completely dissolved, preserving heat for 0.5-2 h, standing for 8-15 h at 5-15 ℃, carrying out suction filtration on a solvent, and vacuum drying the obtained crystal product at 30-50 ℃ for 3-8 h to obtain natural borneol.
The preparation method of the microemulsion comprises the following steps:
s1, adding epichlorohydrin into N, N-dimethylformamide, and stirring to obtain a pretreated substance;
s2, adding carboxymethyl chitosan into a 2-propanol aqueous solution to obtain a mixed solution; adding the pretreated matter prepared in the step S1 into the mixed solution, adding sodium hydroxide aqueous solution for reaction, dialyzing, and freeze-drying to obtain a post-treatment agent;
and S3, adding the post-treatment agent prepared in the step S2 into oleic acid, stirring, adding absolute ethyl alcohol, performing ultrasonic treatment, and filtering to obtain the microemulsion.
Preferably, the preparation method of the microemulsion comprises the following steps in parts by weight:
s1, adding 10-30 parts of epichlorohydrin into 40-60 parts of N, N-dimethylformamide, and stirring at 100-500 rpm for 1-3 hours at the temperature of 40-60 ℃ to obtain a pretreatment substance;
s2, adding 3-8 parts of carboxymethyl chitosan into 80-120 parts of 20-30wt% 2-propanol aqueous solution to obtain a mixed solution; adding the pretreated matter prepared in the step S1 into the mixed solution, adding 5-15 parts of 40-45 wt% sodium hydroxide aqueous solution, reacting for 20-30 hours at 40-60 ℃, finally dialyzing for 1-3 times by using a dialysis bag, wherein the molecular weight cut-off of the dialysis bag is 3-4 kDa, and then freeze-drying for 5-15 hours at-10 to-30 ℃ to obtain a post-treating agent;
s3, adding the post-treatment agent prepared in the step S2 into 3-8 parts of oleic acid, stirring for 1-5 hours at 100-500 rpm, adding 40-60 parts of absolute ethyl alcohol, performing ultrasonic treatment for 10-20 minutes, performing ultrasonic power of 300-500W, performing ultrasonic frequency of 40-60 kHz, and filtering by using a 0.4-0.5 um filter membrane to obtain the microemulsion.
The method for improving sleeping comprises the following steps: dripping 0.3-0.8 mL of herbal composition onto a backing material to prepare the acupoint plaster for improving sleep.
The natural borneol is prepared from fresh branches and leaves of Cinnamomum camphora of Lauraceae by extracting and processing. Has effects of inducing resuscitation, refreshing mind, clearing heat and relieving pain. It is often used for fever, unconsciousness, convulsion, apoplexy, phlegm syncope, qi stagnation syncope, middle-jiao and malignant coma, chest stuffiness and pain, conjunctival congestion, etc.
The Saviae Miltiorrhizae radix extract is dried root and rhizome of Saviae Miltiorrhizae radix of Labiatae. Has effects of promoting blood circulation, removing blood stasis, dredging channels, relieving pain, clearing heart fire, relieving restlessness, cooling blood, and resolving carbuncle. Can be used for treating chest pain, pain in the abdomen and hypochondrium, abdominal mass, pain due to pyretic arthralgia, vexation, insomnia, etc.
The rhizoma Ligustici Chuanxiong extract belongs to pyrazine alkaloids, has effects of dilating blood vessel, increasing arterial blood flow, inhibiting platelet aggregation and platelet activity, promoting qi circulation, promoting blood circulation, dispelling pathogenic wind, relieving pain, and warming and dredging blood vessel.
Stemonae radix is the dried root tuber of Stemonae radix or Stemonae radix. Has effects of moistening lung, descending qi, relieving cough, killing parasite and killing lice. Is commonly used for treating chronic cough, tuberculosis cough and tussiculation; is externally applied to head lice, body lice, enterobiasis and pruritus vulvae. Honey radix stemonae moistens lung to arrest cough, and is used for cough due to yin deficiency.
The kuh-seng is a common Chinese medicinal material, can be used for clearing heat and detoxicating, relieving itching of eczema and the like, and can also be used as an external medicament, such as a lotion, a spray and the like, for treating skin diseases.
Chlorhexidine acetate generally refers to chlorhexidine acetate, which is an organic substance, is white or almost white crystalline powder, and has no odor and bitter taste. Dissolved in ethanol and slightly dissolved in water. The aqueous solution is a medicine for treating colpitis mycotica and cervical erosion, and has the functions of sterilization and disinfection. Can be used for acupoint plaster, is a plaster which is stuck on the acupoint and can relieve symptoms by percutaneous absorption.
The herbal composition is prepared by compounding radix stemonae, radix sophorae flavescentis, radix salviae miltiorrhizae extract, ligusticum chuanxiong hort extract, natural borneol, chlorhexidine acetate, microemulsion, carbomer-940 and water. Wherein the microemulsion is prepared by adding epichlorohydrin into N, N-dimethylformamide and stirring to obtain a pretreatment substance; adding carboxymethyl chitosan into 2-propanol aqueous solution to obtain mixed solution; adding the pretreated matter prepared in the step S1 into the mixed solution, then dropwise adding sodium hydroxide aqueous solution for reaction, dialyzing, and freeze-drying to obtain a post-treatment agent; adding the post-treatment agent into oleic acid, stirring, adding absolute ethyl alcohol, performing ultrasonic treatment, and filtering to obtain the product. The herbal composition is applied to the Shanzhong acupoint by tearing off release paper and dripping into the Chinese medicinal patch.
According to the invention, the hydrophilic carboxymethyl chitosan is successfully prepared by introducing the hydrophobic segment into the hydrophilic carboxymethyl chitosan, and the addition of the pretreatment can increase the hydrophobic interaction between hydrophobic groups, so that a denser hydrophobic core is formed, and therefore, the more the hydrophobic substitution is, the stronger the emulsifying capacity is. Emulsifying ability and lowering surface tension are important properties of surfactants. The functional molecules are dispersed and coated by the microemulsion, and the nano-sized microemulsion can more easily permeate the skin through cell gaps and skin attachments, so that the aim of transdermal drug delivery is fulfilled.
However, storage time is reduced due to poor water solubility, susceptibility to degradation, and instability under light of the functional ingredients in the herbal composition. The microemulsion has good stability after dispersion coating, and the coating layer can be used as a physical barrier for oxygen to prevent the functional components from being oxidized under illumination and enhance the photostability of the functional components. The herbal composition prepared by adding carbomer-940 has certain pseudoplasticity, and is beneficial to be spread on the surface of skin to form a thin layer, and is contacted with the skin for a long time. The medicine remained on the surface of the skin can enter the skin in a transdermal way, thereby achieving the purpose of enhancing the curative effect.
The invention takes the amphipathic carboxymethyl chitosan as the surfactant to prepare a microemulsion system, the system has the functions of nano structure and physical barrier, the solubility and stability of functional molecules are improved, and the microemulsion system effectively promotes the transdermal efficiency of the functional molecules through the interaction with skin appendages (such as hair follicles and sweat glands). Meanwhile, due to the good biocompatibility of the amphipathic chitosan, the microemulsion system does not damage the skin structure and cause erythema, and the skin compatible herbal composition can enhance the treatment effect of functional molecules and promote the improvement of sleep and chest distress.
Compared with the prior art, the invention has the beneficial effects that:
1) The herbal composition is prepared by compounding stemona root, kuh-seng, red sage root extract, szechuan lovage rhizome extract, natural borneol, chlorhexidine acetate, microemulsion, carbomer-940 and water, and can achieve the effects of warming channels and activating collaterals, relieving angina pectoris, relieving coronary heart disease, promoting sleep, refreshing brain and the like by being matched with acupoint patches.
2) According to the invention, the hydrophilic carboxymethyl chitosan is introduced with the hydrophobic segment, so that the amphiphilic carboxymethyl chitosan is successfully prepared, a microemulsion system is further prepared, the solubility and stability of the functional molecules are improved, and the transdermal efficiency of the functional molecules is effectively promoted; at the same time, the microemulsion system does not disrupt skin structure and cause erythema.
3) The acupoint plaster is very convenient to use when being stuck on specific acupoints of a body.
4) The acupoint plaster has quick effect, and the medicinal components of the acupoint plaster can quickly permeate the acupoints and be transferred to focus positions through channels and collaterals, so that the medicinal effect can be quickly exerted.
5) The acupoint plaster has lasting effect, can be continuously pasted on the acupoint for a long time, can continuously permeate the medicinal components, and plays a lasting treatment role.
Detailed Description
The main material sources are as follows:
stemona root: stemona japonica, produced in Hunan Hedyad.
Radix Sophorae Flavescentis: sophora flavescens, produced in shanxi chang zhi.
Root of red-rooted salvia: salvia miltiorrhiza Bunge, produced in the city of Deyang in Sichuan province, zhongjiang county.
Ligusticum wallichii: ligusticum chuanxiong hort, produced in the city of the river of Sichuan.
Borneol camphor tree: dipterocoarpustubennatiusGaertn. F, jiangxi Jian City.
Carboxymethyl chitosan: the model of the Sian super-nation biotechnology Co., ltd: CB.
Example 1
An acupoint patch herbal composition for improving sleep is prepared by the following steps:
step 1, adding 2g of radix stemonae, 2g of radix sophorae flavescentis, 4g of radix salviae miltiorrhizae extract, 4g of ligusticum wallichii extract, 1.5g of natural borneol and 0.1g of chlorhexidine acetate into 8g of microemulsion, and then adding into 40g of water, and stirring at 200rpm for 2 hours to obtain a functional agent;
step 2, adding 1.5g carbomer-940 into 36.9g water, standing overnight, then adding 20wt% potassium bicarbonate aqueous solution to adjust pH to neutral, adding the functional agent prepared in step 1, and stirring at 200rpm for 2h to obtain herbal composition.
The preparation method of the salvia miltiorrhiza extract comprises the following steps:
removing impurities from 1kg of Saviae Miltiorrhizae radix, adding 10kg of water, extracting at 80deg.C for 1 hr, filtering with 100 mesh sieve, adding 6kg of water into the residue, extracting at 80deg.C for 2 times, each time for 0.5 hr, filtering with 100 mesh sieve, mixing the three filtrates, concentrating under reduced pressure at 50deg.C to relative density of 1.05, concentrating under reduced pressure at vacuum degree of 0.09Mpa, and rotating at 50rpm to obtain concentrated solution; cooling to room temperature, adding 0.8kg of 95wt% ethanol water solution, standing for 12h, filtering with a 200-mesh sieve, recovering ethanol to obtain crude drug, and adsorbing with macroporous adsorbent resin AB-8, wherein the mass ratio of crude drug to macroporous adsorbent resin AB-8 is 1:4, washing with water until the effluent liquid has no sugar reaction, and continuing to elute with 40wt% ethanol water solution until the eluent is added with ferric trichloride and potassium ferricyanide reagent to turn green and no precipitate; concentrating the eluate at 50deg.C to relative density of 1.29, and spray drying to obtain Saviae Miltiorrhizae radix extract.
The preparation method of the ligusticum chuanxiong hort extract comprises the following steps:
reflux-extracting 1kg of rhizoma Ligustici Chuanxiong with 5kg of 95wt% ethanol water solution at 70deg.C for 3 times, 90min each time, mixing filtrates, concentrating under reduced pressure to obtain extract, concentrating under reduced pressure at vacuum degree of 0.09Mpa and rotation speed of 50rpm; adding the extract into water with the mass of 5 times, adsorbing with macroporous adsorption resin AB-8, eluting with 30wt% ethanol water solution with the mass of 20 times of the extract, mixing eluates, removing ethanol under reduced pressure, vacuum drying at 40deg.C for 5h under 10kPa to obtain rhizoma Ligustici Chuanxiong extract.
The preparation method of the natural borneol comprises the following steps:
z1, cleaning and drying 2kg of camphora branches and leaves, and then crushing and sieving the camphora branches and leaves by a 40-mesh sieve to obtain camphora branches and leaves powder; adding borneol camphor branch and leaf powder into a 30wt% ethanol water solution with the mass of 8 times, carrying out ultrasonic treatment for 30min at the temperature of 40 ℃ under the ultrasonic power of 500W, filtering by 100 meshes, collecting filtrate, carrying out ultrasonic extraction on residues for 3 times, merging the filtrate, carrying out reduced pressure distillation to form paste, and carrying out reduced pressure concentration at the vacuum degree of 0.09Mpa and the rotating speed of 50rpm to obtain crude natural borneol extract;
z2, the crude extract of the natural borneol prepared in the step Z1 is prepared according to the solid-liquid mass ratio of 1:1.5 vortex 20s after adding tetrahydrofuran-n-octanol-water and centrifuge at 15000rpm for 5min, the mass ratio of tetrahydrofuran, n-octanol and water is 1:1.5:2, pouring out the supernatant, and then, according to the solid-liquid mass ratio of 1:3 adding petroleum ether, stirring and heating in a water bath at 200rpm, keeping the temperature at 50 ℃ for 1h, standing at 10 ℃ for 12h, filtering the solvent, and vacuum drying the obtained crystal product at 40 ℃ for 5h to obtain natural borneol.
The preparation method of the microemulsion comprises the following steps:
s1, adding 20g of epichlorohydrin into 50g of N, N-dimethylformamide, and stirring at 50 ℃ and 200rpm for 2 hours to obtain a pretreatment;
s2, adding 5g of carboxymethyl chitosan into 100g of 25wt% 2-propanol aqueous solution to obtain a mixed solution; adding the pretreated matter prepared in the step S1 into the mixed solution, adding 10g of 42wt% sodium hydroxide aqueous solution, reacting for 24 hours at 50 ℃, finally dialyzing for 3 times by using a dialysis bag, wherein the molecular weight cut-off of the dialysis bag is 4kDa, and then lyophilizing for 10 hours at-20 ℃ to obtain a post-treatment agent;
s3, adding the post-treatment agent prepared in the step S2 into 5g of oleic acid, stirring at 200rpm for 2 hours, adding 50g of absolute ethyl alcohol, performing ultrasonic treatment for 15 minutes, wherein the ultrasonic power is 400W, the ultrasonic frequency is 50kHz, and filtering by using a 0.45um filter membrane to obtain the microemulsion.
The preparation method of the acupoint patch for improving sleep comprises the following steps:
0.5mL of herbal composition is dripped on the backing material to prepare the acupoint plaster for improving sleep.
Example 2
An acupoint patch herbal composition for improving sleep is prepared by the following steps:
step 1, adding 2g of radix stemonae, 2g of radix sophorae flavescentis, 4g of radix salviae miltiorrhizae extract, 4g of ligusticum wallichii extract, 1.5g of natural borneol and 0.1g of chlorhexidine acetate into 8g of microemulsion, and then adding into 40g of water, and stirring at 200rpm for 2 hours to obtain a functional agent;
step 2, adding the functional agent prepared in the step 1 into 36.9g of water, and stirring at 200rpm for 2 hours to obtain the herbal composition.
The preparation method of the salvia miltiorrhiza extract is the same as that of the example 1.
The preparation method of the ligusticum chuanxiong hort extract is the same as that of the example 1.
The preparation method of the natural borneol is the same as that of the example 1.
The preparation of the microemulsion was the same as in example 1.
The preparation method of the acupoint patch for improving sleep is the same as that of the embodiment 1.
Example 3
The preparation method of the herbal composition for acupoint application for improving sleep is basically the same as that of example 1, and the only difference is that: the preparation methods of the microemulsions are different.
The preparation method of the microemulsion comprises the following steps:
s1, adding 5g of carboxymethyl chitosan into 100g of 25wt% 2-propanol aqueous solution to obtain a mixed solution; adding 10g of 42wt% sodium hydroxide aqueous solution, reacting for 24 hours at 50 ℃, finally dialyzing for 3 times by using a dialysis bag, wherein the molecular weight cut-off of the dialysis bag is 4kDa, and then freeze-drying for 10 hours at-20 ℃ to obtain a post-treatment agent;
s2, adding the post-treatment agent prepared in the step S1 into 5g of oleic acid, stirring at 200rpm for 2 hours, adding 50g of absolute ethyl alcohol, performing ultrasonic treatment for 15 minutes, wherein the ultrasonic power is 400W, the ultrasonic frequency is 50kHz, and filtering by using a 0.45um filter membrane to obtain the microemulsion.
The preparation method of the salvia miltiorrhiza extract is the same as that of the example 1.
The preparation method of the ligusticum chuanxiong hort extract is the same as that of the example 1.
The preparation method of the natural borneol is the same as that of the example 1.
The preparation method of the acupoint patch for improving sleep is the same as that of the embodiment 1.
Example 4
The preparation method of the herbal composition for acupoint application for improving sleep is basically the same as that of example 1, and the only difference is that: the preparation methods of the microemulsions are different.
The preparation method of the microemulsion comprises the following steps:
s1, adding 20g of epichlorohydrin into 50g of N, N-dimethylformamide, and stirring at 50 ℃ and 200rpm for 2 hours to obtain a pretreatment;
s2, adding 5g of carboxymethyl chitosan into 100g of 25wt% 2-propanol aqueous solution to obtain a mixed solution; adding the pretreated matter prepared in the step S1 into the mixed solution, adding 10g of 42wt% sodium hydroxide aqueous solution, reacting for 24 hours at 50 ℃, finally dialyzing for 3 times by using a dialysis bag, wherein the molecular weight cut-off of the dialysis bag is 4kDa, and then lyophilizing for 10 hours at-20 ℃ to obtain a post-treatment agent;
s3, adding 50g of absolute ethyl alcohol into the post-treatment agent prepared in the step S2, performing ultrasonic treatment for 15min, wherein the ultrasonic power is 400W, the ultrasonic frequency is 50kHz, and filtering by using a 0.45um filter membrane to obtain the microemulsion.
The preparation method of the salvia miltiorrhiza extract is the same as that of the example 1.
The preparation method of the ligusticum chuanxiong hort extract is the same as that of the example 1.
The preparation method of the natural borneol is the same as that of the example 1.
The preparation method of the acupoint patch for improving sleep is the same as that of the embodiment 1.
Comparative example 1
The preparation method of the herbal composition for acupoint application for improving sleep is basically the same as that of example 1, and the only difference is that: the preparation methods of the herbal composition for acupoint application and the microemulsion are different.
An acupoint patch herbal composition for improving sleep is prepared by the following steps:
step 1, adding 2g of radix stemonae, 2g of radix sophorae flavescentis, 4g of radix salviae miltiorrhizae extract, 4g of ligusticum wallichii extract, 1.5g of natural borneol and 0.1g of chlorhexidine acetate into 8g of microemulsion, and then adding into 40g of water, and stirring at 200rpm for 2 hours to obtain a functional agent;
step 2, adding the functional agent prepared in the step 1 into 36.9g of water, and stirring at 200rpm for 2 hours to obtain the herbal composition.
The preparation method of the microemulsion comprises the following steps:
s1, adding 5g of carboxymethyl chitosan into 100g of 25wt% 2-propanol aqueous solution to obtain a mixed solution; adding 10g of 42wt% sodium hydroxide aqueous solution, reacting for 24 hours at 50 ℃, finally dialyzing for 3 times by using a dialysis bag, wherein the molecular weight cut-off of the dialysis bag is 4kDa, and then freeze-drying for 10 hours at-20 ℃ to obtain a post-treatment agent;
s2, adding 50g of absolute ethyl alcohol into the post-treatment agent prepared in the step S1, performing ultrasonic treatment for 15min, wherein the ultrasonic power is 400W, the ultrasonic frequency is 50kHz, and filtering by using a 0.45um filter membrane to obtain the microemulsion.
The preparation method of the salvia miltiorrhiza extract is the same as that of the example 1.
The preparation method of the ligusticum chuanxiong hort extract is the same as that of the example 1.
The preparation method of the natural borneol is the same as that of the example 1.
The preparation method of the acupoint patch for improving sleep is the same as that of the embodiment 1.
Comparative example 2
The preparation method of the herbal composition for acupoint application for improving sleep is basically the same as that of example 1, and the only difference is that: the preparation method of the herbal composition for acupoint application is free from microemulsion.
The preparation method of the salvia miltiorrhiza extract is the same as that of the example 1.
The preparation method of the ligusticum chuanxiong hort extract is the same as that of the example 1.
The preparation method of the natural borneol is the same as that of the example 1.
The preparation method of the acupoint patch for improving sleep is the same as that of the embodiment 1.
Test example 1
Test for improving sleep effect
The method comprises the steps of selecting 70 volunteers with ages of 20-40 years old, randomly dividing the faces of the volunteers into 7 groups, wherein each group comprises 10 people, each group corresponds to acupoint patches prepared in tested examples and comparative examples, cleaning corresponding acupoints by using clear water as a blank control group, firstly kneading the corresponding acupoints with thumbs in sequence, enabling the strength to be light to heavy from small to large within 1-2 minutes, and applying the acupoint patches prepared by the invention to Shanzhong acupoints after searching sensitive points. The product is applied once every night, taken down in the morning and continuously used for 7 days, and other products for improving the sleeping effect are not used in the period; and after 7 days of use, evaluating the curative effect of the product by adopting a scoring system, wherein the sleep improvement condition is that the score is 10 minutes, the score is higher, the sleep improvement restoration effect is better, the average score is calculated, and the average score of each symptom is calculated to count the average effect of the test sample. The test results are shown in Table 1.
Table 1: test result for improving sleep effect after continuous use for 7 days
Test example 2
Test for improving chest distress effect
The testing method comprises the following steps: 130 volunteers are randomly selected, the ages of 20-60 years, the volunteers are randomly divided into 13 groups, 10 persons in each group are taken as a blank control group, the herbal composition of the test sample of the invention and the herbal composition of the comparison example are irradiated for 12 hours under an ultraviolet lamp, the power of the ultraviolet lamp is 300W, the herbal composition after ultraviolet irradiation and without irradiation is dripped into the acupoint patch, the dripping amount is 0.5mL, and the patch is applied to the Shanzhong acupoint. The plaster is applied once every night, taken down in the morning and continuously used for 15 days, and other products for improving chest distress effect are not used in the period; the chest distress relieving effect is statistically improved by inquiring the chest distress relieving condition, and is classified into the indexes of obvious effect, good effect, partial effective, general effect and ineffective, and the chest distress relieving effect is evaluated, and the test results are shown in table 2.
Table 2: test result for improving chest distress effect
As can be seen from the test results of test examples 1 and 2, the use effect of example 1 is best among the examples and comparative examples, probably because the amphiphilic carboxymethyl chitosan is successfully prepared by introducing the hydrophobic segment into the hydrophilic carboxymethyl chitosan, and the addition of the pretreatment can increase the hydrophobic interaction between the hydrophobic groups, thereby forming a denser hydrophobic core, so that the more hydrophobic substitution is, the stronger the emulsifying ability is. Emulsifying ability and lowering surface tension are important properties of surfactants. The functional molecules are dispersed and coated by the microemulsion, and the nano-sized microemulsion can more easily permeate the skin through cell gaps and skin attachments, so that the aim of transdermal drug delivery is fulfilled.
However, storage time is reduced due to poor water solubility, susceptibility to degradation, and instability under light of the functional ingredients in the herbal composition. The microemulsion has good stability after dispersion coating, and the coating layer can be used as a physical barrier for oxygen to prevent the functional components from being oxidized under illumination and enhance the photostability of the functional components. Herbal compositions are prepared by adding carbomer-940. The herbal composition has certain pseudoplasticity, and is beneficial to be spread on the surface of skin to form a thin layer, and is contacted with the skin for a long time. The medicine remained on the surface of the skin can enter the skin in a transdermal way, thereby achieving the purpose of enhancing the curative effect. Therefore, the treatment effect of example 1 is best, and the treatment effect is still better after ultraviolet irradiation.
Claims (9)
1. An acupoint application herbal composition for improving sleep is characterized by comprising the following raw materials: radix Stemonae, radix Sophorae Flavescentis, saviae Miltiorrhizae radix extract, rhizoma Ligustici Chuanxiong extract, natural Borneolum, chlorhexidine acetate, microemulsion, carbomer-940, and water.
2. The herbal composition for acupoint application for improving sleep of claim 1, which comprises the following raw materials in percentage by weight: 1 to 3 percent of radix stemonae, 1 to 3 percent of radix sophorae flavescentis, 2 to 5 percent of radix salviae miltiorrhizae extract, 2 to 5 percent of rhizoma ligustici wallichii extract, 1 to 2 percent of natural borneol, 0.01 to 0.3 percent of chlorhexidine acetate, 5 to 10 percent of microemulsion, 1 to 2 percent of carbomer-940 and 100 percent of water.
3. The herbal composition for acupoint application for improving sleep as claimed in claim 1 or 2, wherein the preparation method of the extract of red sage root is as follows: removing impurities from radix salviae miltiorrhizae, adding water with the mass of 8-12 times, heating and extracting for 0.5-3 h at 60-90 ℃, filtering by a sieve with 50-200 meshes, reserving filtrate, adding water with the mass of 4-8 times into dregs, heating and extracting for 1-3 times at 60-90 ℃, filtering by a sieve with 50-200 meshes each time, merging filtrate, concentrating under reduced pressure at 40-60 ℃ until the relative density is 1.03-1.06, concentrating under reduced pressure at the vacuum degree of 0.08-0.095 Mpa, and rotating at 30-100 rpm to obtain concentrated solution; cooling to room temperature, adding 80-95 wt% ethanol water solution with the mass of 0.8 times, standing for 5-24 h, filtering by a 100-300 mesh sieve, recovering ethanol to obtain crude drug, adsorbing by macroporous adsorption resin AB-8, wherein the mass ratio of the crude drug to the macroporous adsorption resin AB-8 is 1: 2-5, washing with water until effluent liquid has no sugar reaction, and continuing to use 20-50wt% ethanol water solution for elution until the eluent is added with ferric trichloride and potassium ferricyanide reagent to turn green and no precipitation; concentrating the eluent at 40-60 ℃ until the relative density is 1.25-1.3, and spray drying to obtain the salvia miltiorrhiza extract.
4. The herbal composition for acupoint application for improving sleep according to claim 1 or 2, wherein the preparation method of the ligusticum chuanxiong hort extract is as follows: reflux-extracting rhizoma Ligustici Chuanxiong with 3-7 times of 80-95wt% ethanol water solution at 60-80deg.C for 1-3 times, 50-100 min each time, mixing filtrates, concentrating under reduced pressure to obtain extract, concentrating under reduced pressure at vacuum degree of 0.08-0.095 Mpa and rotation speed of 30-100 rpm; adding the extract into water with the mass of 3-7 times, adsorbing by using macroporous adsorption resin AB-8, eluting by using 20-40 wt% ethanol water solution with the mass of 15-25 times of the extract, combining the eluates, removing ethanol under reduced pressure, drying in vacuum for 3-8 hours at the temperature of 30-50 ℃ to obtain the ligusticum chuanxiong hort extract.
5. The herbal composition for acupoint application for improving sleep as claimed in claim 1 or 2, wherein the preparation method of the natural borneol is as follows:
z1, cleaning and drying branches and leaves of borneol camphor trees, and then crushing the branches and leaves of borneol camphor trees and sieving the crushed branches and leaves of borneol camphor trees with a 30-100-mesh sieve to obtain borneol camphor branch and leaf powder; adding borneol camphor branch and leaf powder into an ethanol water solution with the mass of 20-40 wt% which is 5-10 times, carrying out ultrasonic treatment for 20-40 min at the temperature of 30-50 ℃ under the ultrasonic power of 400-600W, filtering with 50-200 meshes, collecting filtrate, carrying out ultrasonic extraction on residues for 1-3 times, merging the filtrate, carrying out reduced pressure distillation to form paste, carrying out reduced pressure concentration, wherein the vacuum degree is 0.08-0.095 Mpa, and the rotating speed is 30-100 rpm, thus obtaining crude natural borneol extract;
z2, the crude extract of the natural borneol prepared in the step Z1 is prepared according to the solid-liquid mass ratio of 1:1 to 3, adding tetrahydrofuran-n-octanol-water, then swirling for 10 to 30 seconds, centrifuging for 3 to 8 minutes at 10000 to 20000rpm, wherein the mass ratio of the tetrahydrofuran, the n-octanol and the water is 0.8 to 1.2: 1-2: 1.5 to 2.5, and after the supernatant is poured off, the solid-liquid mass ratio is 1: adding petroleum ether into 2-4 parts, putting into a water bath kettle, stirring and heating at 100-500 rpm, heating at 40-60 ℃ until the petroleum ether is completely dissolved, preserving heat for 0.5-2 h, standing for 8-15 h at 5-15 ℃, carrying out suction filtration on a solvent, and vacuum drying the obtained crystal product at 30-50 ℃ for 3-8 h to obtain natural borneol.
6. The herbal composition for acupoint application for improving sleep as claimed in claim 1 or 2, wherein the microemulsion is prepared by the following method:
s1, adding epichlorohydrin into N, N-dimethylformamide, and stirring to obtain a pretreated substance;
s2, adding carboxymethyl chitosan into a 2-propanol aqueous solution to obtain a mixed solution; adding the pretreated matter prepared in the step S1 into the mixed solution, adding sodium hydroxide aqueous solution for reaction, dialyzing, and freeze-drying to obtain a post-treatment agent;
and S3, adding the post-treatment agent prepared in the step S2 into oleic acid, stirring, adding absolute ethyl alcohol, performing ultrasonic treatment, and filtering to obtain the microemulsion.
7. The herbal composition for acupoint application for improving sleep of claim 6, wherein the microemulsion is prepared by the following steps in parts by weight:
s1, adding 10-30 parts of epichlorohydrin into 40-60 parts of N, N-dimethylformamide, and stirring at 100-500 rpm for 1-3 hours at the temperature of 40-60 ℃ to obtain a pretreatment substance;
s2, adding 3-8 parts of carboxymethyl chitosan into 80-120 parts of 20-30wt% 2-propanol aqueous solution to obtain a mixed solution; adding the pretreated matter prepared in the step S1 into the mixed solution, adding 5-15 parts of 40-45 wt% sodium hydroxide aqueous solution, reacting for 20-30 hours at 40-60 ℃, finally dialyzing for 1-3 times by using a dialysis bag, wherein the molecular weight cut-off of the dialysis bag is 3-4 kDa, and then freeze-drying for 5-15 hours at-10 to-30 ℃ to obtain a post-treating agent;
s3, adding the post-treatment agent prepared in the step S2 into 3-8 parts of oleic acid, stirring for 1-5 hours at 100-500 rpm, adding 40-60 parts of absolute ethyl alcohol, performing ultrasonic treatment for 10-20 minutes, performing ultrasonic power of 300-500W, performing ultrasonic frequency of 40-60 kHz, and filtering by using a 0.4-0.5 um filter membrane to obtain the microemulsion.
8. A process for preparing a herbal composition as claimed in any one of claims 1 to 7, characterized by the steps of:
step 1, weighing the raw materials according to the weight percentage, adding radix stemonae, radix sophorae flavescentis, radix salviae miltiorrhizae extract, ligusticum wallichii extract, natural borneol and chlorhexidine acetate into the microemulsion, then adding the mixture into water, and stirring at 100-500 rpm for 1-3 hours to obtain a functional agent;
and 2, adding carbomer-940 into water, standing overnight, adding 10-22 wt% potassium bicarbonate aqueous solution to adjust the pH to be neutral, adding the functional agent prepared in the step 1, and stirring at 100-500 rpm for 1-3 h to obtain the herbal composition.
9. A method for preparing an acupoint patch for improving sleep using the herbal composition as claimed in any one of claims 1 to 7, wherein the steps are as follows: dripping 0.3-0.8 mL of herbal composition as claimed in any one of claims 1-7 onto a backing material to obtain the acupoint plaster for improving sleep.
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