CN113274444A - Plaster for treating bronchial asthma and preparation method thereof - Google Patents
Plaster for treating bronchial asthma and preparation method thereof Download PDFInfo
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- A61K36/18—Magnoliophyta (angiosperms)
- A61K36/88—Liliopsida (monocotyledons)
- A61K36/888—Araceae (Arum family), e.g. caladium, calla lily or skunk cabbage
- A61K36/8888—Pinellia
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Abstract
The invention discloses a plaster for treating bronchial asthma and a preparation method thereof, and the plaster comprises a back lining layer, a plaster layer and a protective layer which are sequentially attached; the ointment layer comprises Chinese medicinal extract and hydrogel matrix; the traditional Chinese medicine extract comprises the following components in parts by weight: 1-2 parts of ginger processed pinellia, 1-2 parts of flos farfarae, 1.5-2.5 parts of semen brassicae, 1.5-2.5 parts of ephedra, 0.5-1.5 parts of cinnamon, 2-3 parts of rhizoma corydalis, 1-2 parts of asarum, 1-2 parts of schisandra chinensis, 1-2 parts of clove and 1-3 parts of euphorbia kansui; the components of the hydrogel matrix comprise: sodium carboxymethylcellulose, a polydopamine-modified metal organic framework material, gluconolactone, a humectant and a transdermal enhancer. The invention adopts the modified hydrogel as the plaster substrate, avoids the inactivation of the traditional Chinese medicine components in the preparation process of the plaster, reduces the irritation of the plaster to the human body, and the prepared plaster has good medicine release property, proper viscosity and difficult residue on the skin.
Description
Technical Field
The invention relates to the technical field of traditional Chinese medicine plaster, in particular to a plaster for treating bronchial asthma and a preparation method thereof.
Background
Bronchial asthma is a chronic airway inflammation involving various cells and cell components, which is often accompanied by increased airway responsiveness, resulting in recurrent wheezing, shortness of breath, chest tightness, and cough, which often occur at night or early in the morning, with a wide and variable airflow obstruction that can be reversed either by itself or by therapy. Asthma is one of the most common chronic diseases in the world at present, is caused by a plurality of viruses or bacteria, is a difficult miscellaneous disease, a common disease and a frequently encountered disease, and is more serious in mental pain caused by the disease than the disease per se, so that the asthma becomes a chronic respiratory disease seriously harming the health of people.
At present, modern medicine has no cure method for asthma, western medicine mainly adopts methods of oxygen inhalation, anti-inflammation, anti-infection, sedation, respiratory tract humidification and the like in the treatment of asthma, wherein glucocorticoid inhalation is one of the most common and basic methods with better clinical effect in the treatment, and as is well known, hormone medicines are easy to cause various local or systemic adverse reactions after long-term use, thus being not beneficial to human health. Asthma is generalized to the category of 'asthma syndrome' in the theory of traditional Chinese medicine, and is considered to be caused by phlegm turbidity blocking an airway and lung qi ascending and descending disadvantages, the asthma can be induced by mental stimulation, wind-cold invasion and the like, more researches in clinic are internal treatment methods of traditional Chinese medicine oral preparations, and the oral preparations have first-pass effect inevitably.
The absorption and metabolism of the externally applied medicine are completely different from those of oral medicine, and the externally applied medicine reaches the interior of the body through the osmosis of the skin, so that the first pass effect of the liver and the degradation of the medicine in the gastrointestinal tract can be avoided, the individual difference of the medicine can be reduced, the peak valley phenomenon of blood concentration caused by oral administration and the like can be avoided, and the toxic and side effects are reduced, so that the Chinese medicinal emplastrum for treating asthma is widely concerned. For example, the patent literature of Chinese discloses "a Chinese medicinal plaster for external use for treating cough and asthma", which is published under the publication No. CN106798877A, and the plaster is composed of 23 kinds of raw material medicines such as perilla stem, grassleaf sweelflag rhizome, Japanese Aristolochia, kaempferia galangal, fructus galangae, pubescent holly root, medicated leaven, radish seed, magnolia bark, villous amomum fruit, sweetgum resin and the like.
However, the traditional plaster generally adopts hot melt adhesive as a matrix, the traditional Chinese medicine components can be added after the hot melt adhesive is dissolved at high temperature, and most of the traditional Chinese medicine active ingredients lose activity under the action of high temperature, so the curative effect is limited; the hot melt adhesive has high viscosity, so that body hair is easy to stick when the plaster is peeled off, and pain of a patient is caused; the hot melt adhesive plaster has no air permeability when being applied, is easy to remain on the skin after being torn off, and has larger irritation to the skin, so that the skin of a patient is easy to have hyperemia, burning heat, pruritus and other anaphylactic reactions after being applied.
Disclosure of Invention
The invention aims to overcome the defects that the bronchial asthma plaster in the prior art generally adopts hot melt adhesive as a matrix, and the traditional Chinese medicine components of the hot melt adhesive plaster are easy to inactivate at high temperature in the processing process to influence the curative effect; the plaster for treating bronchial asthma is prepared by using hydrogel modified by polydopamine-modified metal organic framework material as a matrix, and the traditional Chinese medicine components for treating bronchial asthma are prepared into the cataplasm plaster, so that the inactivation of the traditional Chinese medicine components in the plaster preparation process is avoided, the irritation of the plaster to a human body is reduced, and the prepared plaster has good medicine release property, proper viscosity and is not easy to remain on skin.
In order to achieve the purpose, the invention adopts the following technical scheme:
a plaster for treating bronchial asthma comprises a back lining layer, a plaster layer and a protective layer which are sequentially attached; the raw materials of the plaster layer comprise a traditional Chinese medicine extract and a hydrogel matrix in a mass ratio of 1: 5-7; the traditional Chinese medicine extract comprises the following components in parts by weight: 1-2 parts of ginger processed pinellia, 1-2 parts of flos farfarae, 1.5-2.5 parts of semen brassicae, 1.5-2.5 parts of ephedra, 0.5-1.5 parts of cinnamon, 2-3 parts of rhizoma corydalis, 1-2 parts of asarum, 1-2 parts of schisandra chinensis, 1-2 parts of clove and 1-3 parts of euphorbia kansui; the components of the hydrogel matrix comprise the following components in parts by weight: 25-35 parts of sodium carboxymethylcellulose, 20-30 parts of polydopamine-modified metal organic framework material, 5-10 parts of glucolactone, 20-40 parts of humectant and 5-10 parts of transdermal enhancer.
The plaster of the invention is compounded by a plurality of traditional Chinese medicine components, and the ginger processed pinellia tuber enters the stomach channel, can eliminate phlegm-dampness of middle-jiao and can also increase the transportation and transformation capacity of spleen and stomach; flos Farfarae has effects of moistening lung, descending qi, relieving cough, eliminating phlegm, and relieving asthma; semen Sinapis Albae has effects of activating qi-flowing, eliminating phlegm, warming spleen and stomach, dispelling cold, dredging collaterals and relieving pain; the ephedra herb is helpful for sweating, relieving asthma and inducing diuresis, and is used for treating typhoid fever, exterior excess, fever, aversion to cold and anhidrosis; the herba asari has effects of dispelling pathogenic wind, dispelling cold, promoting diuresis, and inducing resuscitation; gan Tuo has the effects of purging water, dispersing fluid retention, relieving swelling and dissipating stagnation; under the synergistic effect of the components, the plaster of the invention has good effects of ventilating the lung, lowering qi, reducing phlegm, relieving cough and asthma and has better curative effect on bronchial asthma.
Meanwhile, in order to reduce the irritation of the plaster to a human body, the hydrogel is used as a plaster substrate, and the hydrogel has good water retention capacity, soft and elastic structure, is not adhered and pulled with skin and wounds, and has no irritation to biological substrates, so the plaster prepared by using the hydrogel as the substrate is nontoxic and non-irritant, has good compatibility with the skin, and is not easy to cause allergy after being applied; and has good moisture retention and certain slow release effect on the medicine. However, the existing hydrogel matrix has the problems of poor strength and incapability of considering both cohesion and viscosity: when the crosslinking degree of the matrix is higher, the viscosity of the matrix is poor, and the plaster is easy to fall off during application; when the matrix is not completely crosslinked, although the matrix has better initial viscosity, the cohesive force is poor, the forming property does not meet the requirement, and the phenomenon of paste removal is easy to occur; and the three-dimensional network structure is not completely formed, and the water retentivity is lowered, so that the proper adhesiveness cannot be maintained for a long time.
Therefore, the hydrogel matrix is modified by the polydopamine-modified metal-organic framework material, the metal-organic framework material is a coordination polymer with a three-dimensional pore structure and formed by metal ions and organic ligands, the hydrogel is modified by the metal-organic framework material, the strength of the matrix can be effectively improved, and the hydrogel can adsorb traditional Chinese medicine components due to the characteristics of the porous structure and high porosity, so that the traditional Chinese medicine components have slow release performance, and the action time of the plaster is prolonged. The polydopamine is a material without irritation source for organisms with good adhesion characteristics, and the polydopamine is used for modifying a metal organic framework material and modifying a hydrogel matrix together, so that the viscosity of the matrix can be greatly improved. After the polydopamine modified metal organic framework material and the sodium carboxymethyl cellulose are mixed, a block polymer of the polydopamine modified metal organic framework material and the sodium carboxymethyl cellulose can be formed under the action of hydrogen bonds of amino groups in the polydopamine modified metal organic framework material and carboxyl groups in the sodium carboxymethyl cellulose, and then under the aggregation action of a metal organic framework nano material, hydrogel with a three-dimensional network structure is formed; the hydrogel matrix formed in the invention has good strength and cohesion, good forming property, good water retention and moisture retention, and high viscosity, so that the plaster can be firmly applied.
Preferably, the preparation method of the polydopamine modified metal organic framework material comprises the following steps:
A) dispersing zinc chloride and 2-amino-terephthalic acid in a solvent, stirring for dissolving, sequentially adding o-methyl-benzyl and hydrochloric acid, carrying out hydrothermal reaction at 140-160 ℃ for 10-15 h, carrying out centrifugal separation, washing, drying and crushing a product to obtain an amino-modified metal organic framework material;
B) adding the metal organic framework material modified by the amino into toluene, adding a dopamine solution after the metal organic framework material is uniformly dispersed, uniformly stirring, adjusting the pH value of a system to 8-9, and carrying out water bath reaction at 90-100 ℃ for 18-36 hours to obtain the metal organic framework material modified by the polydopamine.
When the polydopamine modified metal organic framework material is prepared, firstly, the step A) is carried out, and 2-amino-terephthalic acid with amino is taken as a ligand to prepare the amino modified metal organic framework material; and then through the step B), carrying out Michael addition reaction on amino in the metal organic framework material and quinone group generated after dopamine self-polymerization in an alkaline environment, so as to connect polydopamine on the metal organic framework material, wherein the obtained polydopamine modified metal organic framework material has abundant amino on the surface, and can form hydrogen bond action with carboxyl in sodium carboxymethylcellulose to form a block polymer, thereby further forming the hydrogel with a three-dimensional network structure.
Preferably, the mass ratio of the zinc chloride, the 2-amino-terephthalic acid and the o-methylbenzoic acid in the step A) is 1: 1-2; the addition amount of the hydrochloric acid is 1-3% of the total mass of the solution.
Preferably, the mass ratio of the amino-modified metal organic framework material in the step B) to the added dopamine is 1: 3-4.
Preferably, the humectant is one or more selected from glycerol, propylene glycol, ethylene glycol, diethylene glycol, polyethylene glycol, sorbitol and 1, 3-butanediol; the skin penetration enhancer is selected from one or more of azone, menthol, Borneolum Syntheticum, oleum Eucalypti, oleum Terebinthinae, salicylic acid, oleic acid, and lauryl alcohol.
Preferably, the backing layer is a non-woven fabric, and the protective layer is one selected from release paper, a polyethylene film and a polypropylene film.
The invention also provides a preparation method of the plaster, which comprises the following steps:
(1) preparing a traditional Chinese medicine extract;
(2) dispersing the metal organic framework material modified by polydopamine in water to obtain a dispersion liquid, uniformly stirring and dispersing, adjusting the pH value of the dispersion liquid to 11-12, then adding the dispersion liquid into an aqueous solution of sodium carboxymethylcellulose, stirring for 40-60 min, and then adding a glucolactone solution;
(3) adding the traditional Chinese medicine extract, the humectant and the transdermal enhancer into the system obtained in the step (2), and stirring for 30-40 min to obtain a paste layer raw material;
(4) and coating the raw materials of the plaster layer on the surface of the back lining layer, standing for 6-8 h for curing, covering a protective layer, and cutting to obtain the plaster.
Preferably, the preparation method of the traditional Chinese medicine extract in the step (1) comprises the following steps: crushing the traditional Chinese medicinal materials, adding the crushed traditional Chinese medicinal materials into an ethanol solution, carrying out reflux extraction for 5-7 h, filtering, adding filter residues into the ethanol solution, continuously carrying out reflux extraction for 2-3 h, combining the filtrates after filtration, and concentrating to obtain clear paste with the relative density of 1.15-1.25 at 60 ℃.
Preferably, the mass concentration of the ethanol solution is 60-70%, and the mass ratio of the traditional Chinese medicine powder to the ethanol solution in the reflux extraction is 1: 6-8.
Preferably, the mass concentration of the polydopamine modified metal organic framework material in the dispersion liquid in the step (2) is 10-15%, and the mass concentration of the sodium carboxymethyl cellulose aqueous solution is 3-5%; the mass concentration of the gluconolactone solution is 10-20%.
Therefore, the invention has the following beneficial effects:
(1) the hydrogel is used as a plaster substrate, and the prepared plaster is non-toxic, non-irritant, good in compatibility with skin and not easy to be allergic after application; the moisture retention is good, and the sustained-release tablet has a certain sustained-release effect on the medicine;
(2) the hydrogel matrix is modified by the polydopamine-modified metal organic framework material, the metal organic framework material can effectively improve the strength of the matrix, and the porous structure and the high porosity of the metal organic framework material can adsorb the traditional Chinese medicine components, so that the traditional Chinese medicine components have slow release performance, the action time of the plaster is prolonged, and the viscosity of the matrix can be greatly improved by the polydopamine;
(3) forming a block polymer of the metal organic framework material modified by the polydopamine and the sodium carboxymethyl cellulose under the action of hydrogen bonds of amino groups in the metal organic framework material modified by the polydopamine and carboxyl groups in the sodium carboxymethyl cellulose, and further forming hydrogel with a three-dimensional network structure under the aggregation action of the metal organic framework nano material; the hydrogel matrix formed in the invention has good strength and cohesion, good forming property, good water retention and moisture retention, and high viscosity.
Detailed Description
The invention is further described with reference to specific embodiments.
In the present invention, all the equipment and materials are commercially available or commonly used in the art, and the methods in the following examples are conventional in the art unless otherwise specified.
Example 1:
a plaster for treating bronchial asthma comprises a back lining layer, a plaster layer and a protective layer which are sequentially attached; the back lining layer adopts non-woven fabrics, the protective layer adopts release paper, and the raw materials of the plaster layer comprise traditional Chinese medicine extract and hydrogel matrix in a mass ratio of 1: 6; the traditional Chinese medicine extract comprises the following components in parts by weight: 1.5 parts of ginger processed pinellia tuber, 1.5 parts of common coltsfoot flower, 2 parts of white mustard seed, 2 parts of ephedra herb, 1 part of cinnamon, 2.5 parts of rhizoma corydalis, 1.5 parts of asarum, 1.5 parts of Chinese magnoliavine fruit, 1.5 parts of clove and 2 parts of kansui root; the components of the hydrogel matrix comprise the following components in parts by weight: 30 parts of sodium carboxymethylcellulose, 25 parts of polydopamine-modified metal organic framework material, 6 parts of glucolactone, 20 parts of glycerol, 10 parts of propylene glycol and 8 parts of azone.
The preparation method of the polydopamine modified metal organic framework material comprises the following steps:
A) dispersing zinc chloride and 2-amino-terephthalic acid in a solvent, stirring for dissolving, and sequentially adding o-methylbenzene and hydrochloric acid, wherein the mass ratio of the zinc chloride to the 2-amino-terephthalic acid to the o-methylbenzoic acid is 1:1.5: 1.5; the addition amount of the hydrochloric acid is 2 percent of the total mass of the solution; carrying out hydrothermal reaction for 12h at 150 ℃, washing, drying and crushing a product after centrifugal separation to obtain an amino-modified metal organic framework material;
B) adding the metal organic framework material modified by amino into toluene, wherein the mass-volume ratio of the metal organic framework material modified by amino to the toluene is 1g:400 mL; and adding a dopamine solution after ultrasonic dispersion is uniform, wherein the mass ratio of the amino modified metal organic framework material to the added dopamine is 1:3.5, uniformly stirring, adjusting the pH value of the system to 8.5 by using a Tris buffer solution, and carrying out water bath reaction at 95 ℃ for 24 hours to obtain the poly-dopamine modified metal organic framework material.
The preparation method of the plaster comprises the following steps:
(1) preparing a traditional Chinese medicine extract: crushing the traditional Chinese medicinal materials, respectively adding the crushed traditional Chinese medicinal materials into 65 wt% ethanol solution, wherein the mass ratio of the traditional Chinese medicinal material powder to the ethanol solution is 1:7, performing reflux extraction for 6 hours, filtering, adding filter residues into the ethanol solution, performing reflux extraction for 2.5 hours by the same method, combining the filtrates obtained after filtration, concentrating to obtain clear paste with the relative density of 1.21 at 60 ℃, and mixing the clear pastes of the components in proportion to obtain the traditional Chinese medicinal extract;
(2) dispersing the polydopamine modified metal organic framework material in water to obtain 12 wt% dispersion, uniformly stirring and dispersing, adjusting the pH of the dispersion to 11.5 by using a NaOH solution, then adding the dispersion into a 4 wt% sodium carboxymethylcellulose aqueous solution according to the mass ratio of the polydopamine modified metal organic framework material to the sodium carboxymethylcellulose, stirring for 50min, and then adding a 15 wt% gluconolactone solution;
(3) adding the traditional Chinese medicine extract, glycerol, propylene glycol and azone into the system obtained in the step (2) in proportion, and stirring for 35min to obtain a paste layer raw material;
(4) coating the paste layer raw material on the surface of the non-woven fabric with the coating weight of 20g/100cm2Standing for 7h for curing, covering with cellophane, and cutting to obtain the plaster.
Example 2:
a plaster for treating bronchial asthma comprises a back lining layer, a plaster layer and a protective layer which are sequentially attached; the back lining layer adopts non-woven fabrics, the protective layer adopts release paper, and the raw materials of the plaster layer comprise traditional Chinese medicine extract and hydrogel matrix in a mass ratio of 1: 5; the traditional Chinese medicine extract comprises the following components in parts by weight: 1 part of pinellia ternate, 1 part of flos farfarae, 1.5 parts of semen brassicae, 1.5 parts of ephedra, 0.5 part of cinnamon, 2 parts of rhizoma corydalis, 1 part of asarum, 1 part of schisandra chinensis, 1 part of clove and 1 part of euphorbia kansui; the components of the hydrogel matrix comprise the following components in parts by weight: 25 parts of sodium carboxymethylcellulose, 20 parts of polydopamine-modified metal organic framework material, 5 parts of glucolactone, 10 parts of glycerol, 10 parts of propylene glycol and 5 parts of azone.
The preparation method of the polydopamine modified metal organic framework material comprises the following steps:
A) dispersing zinc chloride and 2-amino-terephthalic acid in a solvent, stirring for dissolving, and sequentially adding o-methylbenzene and hydrochloric acid, wherein the mass ratio of the zinc chloride to the 2-amino-terephthalic acid to the o-methylbenzoic acid is 1:1: 1; the addition amount of the hydrochloric acid is 1 percent of the total mass of the solution; carrying out hydrothermal reaction for 15h at 140 ℃, washing, drying and crushing a product after centrifugal separation to obtain an amino-modified metal organic framework material;
B) adding the metal organic framework material modified by amino into toluene, wherein the mass-volume ratio of the metal organic framework material modified by amino to the toluene is 1g:300 mL; and adding a dopamine solution after ultrasonic dispersion is uniform, wherein the mass ratio of the amino modified metal organic framework material to the added dopamine is 1:3, uniformly stirring, adjusting the pH value of the system to 8 by using a Tris buffer solution, and carrying out water bath reaction at 90 ℃ for 36 hours to obtain the polydopamine modified metal organic framework material.
The preparation method of the plaster comprises the following steps:
(1) preparing a traditional Chinese medicine extract: pulverizing the traditional Chinese medicinal materials, respectively adding the pulverized traditional Chinese medicinal materials into 60 wt% ethanol solution, wherein the mass ratio of the traditional Chinese medicinal material powder to the ethanol solution is 1:8, refluxing and extracting for 7h, filtering, adding the filter residue into the ethanol solution, continuously refluxing and extracting for 2h by the same method, mixing the two filtrates after filtering, concentrating to obtain a fluid extract with a relative density of 1.15 at 60 ℃, and mixing the fluid extracts of the components in proportion to obtain the traditional Chinese medicine extract;
(2) dispersing the polydopamine modified metal organic framework material in water to obtain 15 wt% of dispersion liquid, stirring and dispersing uniformly, then adjusting the pH value of the dispersion liquid to 11 by using a NaOH solution, then adding the dispersion liquid into a 3 wt% sodium carboxymethylcellulose aqueous solution according to the mass ratio of the polydopamine modified metal organic framework material to the sodium carboxymethylcellulose, stirring for 40min, and then adding a 20 wt% gluconolactone solution;
(3) adding the traditional Chinese medicine extract, glycerol, propylene glycol and azone into the system obtained in the step (2) in proportion, and stirring for 30min to obtain a paste layer raw material;
(4) coating the paste layer raw material on the surface of the non-woven fabric with the coating weight of 20g/100cm2Standing for 6h for curing, covering with cellophane, and cutting to obtain the plaster.
Example 3:
a plaster for treating bronchial asthma comprises a back lining layer, a plaster layer and a protective layer which are sequentially attached; the back lining layer adopts non-woven fabrics, the protective layer adopts release paper, and the raw materials of the plaster layer comprise traditional Chinese medicine extract and hydrogel matrix in a mass ratio of 1: 7; the traditional Chinese medicine extract comprises the following components in parts by weight: 2 parts of pinellia ternate, 2 parts of flos farfarae, 2.5 parts of semen brassicae, 2.5 parts of ephedra, 1.5 parts of cinnamon, 3 parts of rhizoma corydalis, 2 parts of asarum, 2 parts of schisandra chinensis, 2 parts of clove and 3 parts of euphorbia kansui; the components of the hydrogel matrix comprise the following components in parts by weight: 35 parts of sodium carboxymethylcellulose, 30 parts of polydopamine-modified metal organic framework material, 10 parts of glucolactone, 20 parts of glycerol, 20 parts of propylene glycol and 10 parts of azone.
The preparation method of the polydopamine modified metal organic framework material comprises the following steps:
A) dispersing zinc chloride and 2-amino-terephthalic acid in a solvent, stirring for dissolving, and sequentially adding o-methylbenzene and hydrochloric acid, wherein the mass ratio of the zinc chloride to the 2-amino-terephthalic acid to the o-methylbenzoic acid is 1:2: 2; the addition amount of the hydrochloric acid is 3 percent of the total mass of the solution; carrying out hydrothermal reaction for 10h at 160 ℃, washing, drying and crushing a product after centrifugal separation to obtain an amino-modified metal organic framework material;
B) adding the metal organic framework material modified by amino into toluene, wherein the mass-volume ratio of the metal organic framework material modified by amino to the toluene is 1g:500 mL; and adding a dopamine solution after ultrasonic dispersion is uniform, wherein the mass ratio of the amino modified metal organic framework material to the added dopamine is 1:4, uniformly stirring, adjusting the pH value of the system to 9 by using a Tris buffer solution, and carrying out water bath reaction at 100 ℃ for 18h to obtain the polydopamine modified metal organic framework material.
The preparation method of the plaster comprises the following steps:
(1) preparing a traditional Chinese medicine extract: crushing the traditional Chinese medicinal materials, respectively adding the crushed traditional Chinese medicinal materials into 70 wt% ethanol solution, wherein the mass ratio of the traditional Chinese medicinal material powder to the ethanol solution is 1:6, refluxing and extracting for 5 hours, filtering, adding filter residues into the ethanol solution, continuously refluxing and extracting for 3 hours by the same method, mixing the two filtrates after filtering, concentrating to obtain clear paste with the relative density of 1.25 at the temperature of 60 ℃, and mixing the clear pastes of the components in proportion to obtain the traditional Chinese medicinal extract;
(2) dispersing the polydopamine modified metal organic framework material in water to obtain 10 wt% dispersion, uniformly stirring and dispersing, adjusting the pH value of the dispersion to 12 by using a NaOH solution, then adding the dispersion into a 5 wt% sodium carboxymethylcellulose aqueous solution according to the mass ratio of the polydopamine modified metal organic framework material to the sodium carboxymethylcellulose, stirring for 60min, and then adding a 10 wt% gluconolactone solution;
(3) adding the traditional Chinese medicine extract, glycerol, propylene glycol and azone into the system obtained in the step (2) in proportion, and stirring for 40min to obtain a paste layer raw material;
(4) coating the paste layer raw material on the surface of the non-woven fabric with the coating weight of 20g/100cm2Standing for 8h for curing, covering with cellophane, and cutting to obtain the plaster.
Comparative example 1 (no polydopamine modified metal organic framework material added):
the components of the hydrogel matrix in the patch of comparative example 1 were comprised of, in parts by weight: 30 parts of sodium carboxymethylcellulose, 6 parts of glucolactone, 20 parts of glycerol, 10 parts of propylene glycol and 8 parts of azone.
The preparation method of the plaster comprises the following steps:
(1) preparing a traditional Chinese medicine extract: crushing the traditional Chinese medicinal materials, respectively adding the crushed traditional Chinese medicinal materials into 65 wt% ethanol solution, wherein the mass ratio of the traditional Chinese medicinal material powder to the ethanol solution is 1:7, performing reflux extraction for 6 hours, filtering, adding filter residues into the ethanol solution, performing reflux extraction for 2.5 hours by the same method, combining the filtrates obtained after filtration, concentrating to obtain clear paste with the relative density of 1.21 at 60 ℃, and mixing the clear pastes of the components in proportion to obtain the traditional Chinese medicinal extract;
(2) adding 15 wt% of gluconolactone solution into 4 wt% of sodium carboxymethylcellulose aqueous solution;
(3) adding the traditional Chinese medicine extract, glycerol, propylene glycol and azone into the system obtained in the step (2) in proportion, and stirring for 35min to obtain a paste layer raw material;
(4) coating the paste layer raw material on the surface of the non-woven fabric with the coating weight of 20g/100cm2Standing for 7h for curing, covering with cellophane, and cutting to obtain the plaster.
The rest is the same as in example 1.
Comparative example 2 (metal organic framework material not modified with polydopamine):
the components of the hydrogel matrix in the patch of comparative example 2 were comprised of, in parts by weight: 30 parts of sodium carboxymethylcellulose, 25 parts of a metal organic framework material, 6 parts of glucolactone, 20 parts of glycerol, 10 parts of propylene glycol and 8 parts of azone.
The preparation method of the metal organic framework material comprises the following steps: dispersing zinc chloride and 2-amino-terephthalic acid in a solvent, stirring for dissolving, and sequentially adding o-methylbenzene and hydrochloric acid, wherein the mass ratio of the zinc chloride to the 2-amino-terephthalic acid to the o-methylbenzoic acid is 1:1.5: 1.5; the addition amount of the hydrochloric acid is 2 percent of the total mass of the solution; carrying out hydrothermal reaction for 12h at 150 ℃, and washing, drying and crushing a product after centrifugal separation to obtain the metal organic framework material.
The rest is the same as in example 1.
Comparative example 3 (poly dopamine not attached to metal organic framework material):
the components of the hydrogel matrix in the patch of comparative example 3 were comprised of, in parts by weight: 30 parts of sodium carboxymethylcellulose, 5 parts of polydopamine, 20 parts of a metal organic framework material, 6 parts of glucolactone, 20 parts of glycerol, 10 parts of propylene glycol and 8 parts of azone.
The preparation method of the metal organic framework material comprises the following steps: dispersing zinc chloride and 2-amino-terephthalic acid in a solvent, stirring for dissolving, and sequentially adding o-methylbenzene and hydrochloric acid, wherein the mass ratio of the zinc chloride to the 2-amino-terephthalic acid to the o-methylbenzoic acid is 1:1.5: 1.5; the addition amount of the hydrochloric acid is 2 percent of the total mass of the solution; carrying out hydrothermal reaction for 12h at 150 ℃, and washing, drying and crushing a product after centrifugal separation to obtain the metal organic framework material.
The preparation method of the plaster comprises the following steps:
(1) preparing a traditional Chinese medicine extract: crushing the traditional Chinese medicinal materials, respectively adding the crushed traditional Chinese medicinal materials into 65 wt% ethanol solution, wherein the mass ratio of the traditional Chinese medicinal material powder to the ethanol solution is 1:7, performing reflux extraction for 6 hours, filtering, adding filter residues into the ethanol solution, performing reflux extraction for 2.5 hours by the same method, combining the filtrates obtained after filtration, concentrating to obtain clear paste with the relative density of 1.21 at 60 ℃, and mixing the clear pastes of the components in proportion to obtain the traditional Chinese medicinal extract;
(2) dispersing polydopamine and a metal organic framework material in water to obtain a dispersion liquid with the concentration of the metal organic framework material being 12 wt%, stirring and dispersing uniformly, and then adjusting the pH value of the dispersion liquid to 11.5 by using a NaOH solution; then adding the dispersion liquid into 4 wt% of sodium carboxymethyl cellulose aqueous solution according to the mass ratio of the metal organic framework material to the sodium carboxymethyl cellulose, stirring for 50min, and adding 15 wt% of gluconolactone solution;
(3) adding the traditional Chinese medicine extract, glycerol, propylene glycol and azone into the system obtained in the step (2) in proportion, and stirring for 35min to obtain a paste layer raw material;
(4) coating the paste layer raw material on the surface of the non-woven fabric with the coating weight of 20g/100cm2Standing for 7h for curing, covering with cellophane, and cutting to obtain the plaster.
The rest is the same as in example 1.
The patch prepared in the above examples and comparative examples was tested for the application performance and the drug release performance, and the results are shown in tables 1 and 2.
In table 1, the methods for testing initial adhesion, holding adhesion, and peel strength refer to the method for measuring adhesion of XJ patch in the appendix of 2010 edition of chinese pharmacopoeia:
the initial adhesion is measured by a rolling ball slope stopping method, and the set scoring standard is 10 x (10- | A-10|), wherein A represents the number of the steel ball, and the full score is 100; the higher the score is, the better the initial adhesion of the patch meets the quality requirement;
the retention force was scored as follows: measuring the holding power of the sample when the test article is not fallen off at the specified time, wherein s represents the displacement value and the unit is cm; the higher the fraction is, the higher the adhesion force is, the better the quality requirement of the patch is met, and the score is 100;
the peel strength was measured using a 180 ° peel strength test with a rating scale of: peel strength score for the sample 100-F-100, where F represents force value in N; the higher the fraction is, the peel strength meets the quality requirement of the patch, and the full score is 100;
the cohesion and the penetration were determined by sensory evaluation:
cohesion scoring method: placing the prepared sample for 24 hours, wherein the cohesion evaluation is divided into 3 grades, the full score is 100, when the patch attached to the skin is removed, if the patch surface is damaged to cause the matrix to stain the skin, the score is 10-30, and the score is lower when the damage degree is larger; if the paste surface is seriously deformed but the skin is not polluted, the score is 40-70, and the score is lower when the detachment degree is larger; if the cream surface deformation is small and the skin is not stained, the score is 80-100, and the better the cream surface reducibility is, the higher the score is;
and a penetration degree scoring method comprises the following steps: the prepared sample is placed for 24 hours, the back lining layer is not soaked, the permeability is full of 100 minutes, and the higher the soaking degree is, the lower the score is; the higher the fraction is, the more the patch meets the requirements of the patch;
the calculation method of the total evaluation score of the emplastrum comprises the following steps: total score ═ (initial adhesion score + holding adhesion score + peel strength score) × 0.7/3+ (cohesion score + permeability score) × 0.3/2.
Table 1: and testing the application performance of the plaster.
In the test of the drug release performance in table 2, gingerol, an active component in pinellia ternata, is used as a test component, a pig skin is used for establishing a model, the drug release property is measured through a modified Franz diffusion cell, the receiving liquid is normal saline, the temperature of the receiving cell is 32 ℃, the receiving cells are respectively sampled in receiving chambers for 1, 2, 4, 6, 8 and 12 hours, the samples are filtered and analyzed, and the content of the gingerol in the samples is measured by utilizing high performance liquid chromatography.
Table 2: test results of drug release performance of the plaster.
As can be seen from tables 1 and 2, the plasters prepared by the raw materials and the method in the invention in examples 1 to 3 have good initial adhesion, holding adhesion, peeling strength and cohesion, and good application property; and the traditional Chinese medicine components have slow release performance, can be released continuously within 12h, and have lasting drug effect.
In the comparative example 1, the metal-organic framework material modified by polydopamine is not added into the matrix, the sodium carboxymethyl cellulose and the metal-organic framework material modified by polydopamine cannot form hydrogel with a three-dimensional network structure, and the adhesion and cohesion of the plaster are obviously reduced; the adsorbability of the porous structure of the metal organic framework material to the traditional Chinese medicine components is lost, the slow release performance of the medicine is obviously reduced, and the effective components are basically and completely released after 4-6 hours; in comparative example 2, the polydopamine is not modified on the metal organic framework material, and the adhesion and cohesion of the plaster are also reduced compared with those in example 1; in comparative example 3, the poly-dopamine is not connected to the metal-organic framework material, but is directly mixed in the matrix, so that the viscosity and the cohesive force of the plaster are also reduced, and probably because the poly-dopamine is not connected to the metal-organic framework material, when the poly-dopamine is directly mixed, the poly-dopamine cannot participate in the formation of the metal-organic framework material and the carboxymethylcellulose sodium hydrogel, the entanglement of molecular chains in the formed hydrogel is not facilitated, the three-dimensional network structure in the matrix is looser, the cohesive force is reduced, and the use performance of the plaster is influenced.
Claims (10)
1. A plaster for treating bronchial asthma is characterized by comprising a back lining layer, a plaster layer and a protective layer which are sequentially attached; the raw materials of the plaster layer comprise a traditional Chinese medicine extract and a hydrogel matrix in a mass ratio of 1: 5-7; the traditional Chinese medicine extract comprises the following components in parts by weight: 1-2 parts of ginger processed pinellia, 1-2 parts of flos farfarae, 1.5-2.5 parts of semen brassicae, 1.5-2.5 parts of ephedra, 0.5-1.5 parts of cinnamon, 2-3 parts of rhizoma corydalis, 1-2 parts of asarum, 1-2 parts of schisandra chinensis, 1-2 parts of clove and 1-3 parts of euphorbia kansui; the components of the hydrogel matrix comprise the following components in parts by weight: 25-35 parts of sodium carboxymethylcellulose, 20-30 parts of polydopamine-modified metal organic framework material, 5-10 parts of glucolactone, 20-40 parts of humectant and 5-10 parts of transdermal enhancer.
2. The plaster for treating bronchial asthma of claim 1, wherein the preparation method of the polydopamine-modified metal-organic framework material comprises the following steps:
A) dispersing zinc chloride and 2-amino-terephthalic acid in a solvent, stirring for dissolving, sequentially adding o-methyl-benzyl and hydrochloric acid, carrying out hydrothermal reaction at 140-160 ℃ for 10-15 h, carrying out centrifugal separation, washing, drying and crushing a product to obtain an amino-modified metal organic framework material;
B) adding the metal organic framework material modified by the amino into toluene, adding a dopamine solution after the metal organic framework material is uniformly dispersed, uniformly stirring, adjusting the pH value of a system to 8-9, and carrying out water bath reaction at 90-100 ℃ for 18-36 hours to obtain the metal organic framework material modified by the polydopamine.
3. The plaster for treating bronchial asthma according to claim 2, wherein the mass ratio of zinc chloride, 2-amino-terephthalic acid and o-methylbenzoic acid in step a) is 1: 1-2; the addition amount of the hydrochloric acid is 1-3% of the total mass of the solution.
4. The plaster for treating bronchial asthma according to claim 2, wherein the mass ratio of the amino-modified metal organic framework material in step B) to the added dopamine is 1: 3-4.
5. The patch for treating bronchial asthma as claimed in claim 1, wherein said humectant is one or more selected from glycerin, propylene glycol, ethylene glycol, diethylene glycol, polyethylene glycol, sorbitol, 1, 3-butylene glycol; the skin penetration enhancer is selected from one or more of azone, menthol, Borneolum Syntheticum, oleum Eucalypti, oleum Terebinthinae, salicylic acid, oleic acid, and lauryl alcohol.
6. The patch for treating bronchial asthma as claimed in claim 1, wherein said backing layer is non-woven fabric and said protective layer is one selected from release paper, polyethylene film, and polypropylene film.
7. A process for the preparation of a plaster as claimed in any one of claims 1 to 6, comprising the steps of:
(1) preparing a traditional Chinese medicine extract;
(2) dispersing the metal organic framework material modified by polydopamine in water to obtain a dispersion liquid, uniformly stirring and dispersing, adjusting the pH value of the dispersion liquid to 11-12, then adding the dispersion liquid into an aqueous solution of sodium carboxymethylcellulose, stirring for 40-60 min, and then adding a glucolactone solution;
(3) adding the traditional Chinese medicine extract, the humectant and the transdermal enhancer into the system obtained in the step (2), and stirring for 30-40 min to obtain a paste layer raw material;
(4) and coating the raw materials of the plaster layer on the surface of the back lining layer, standing for 6-8 h for curing, covering a protective layer, and cutting to obtain the plaster.
8. The method for preparing the plaster according to claim 7, wherein the method for preparing the Chinese medicinal extract in the step (1) comprises the following steps: crushing the traditional Chinese medicinal materials, adding the crushed traditional Chinese medicinal materials into an ethanol solution, carrying out reflux extraction for 5-7 h, filtering, adding filter residues into the ethanol solution, continuously carrying out reflux extraction for 2-3 h, combining the filtrates after filtration, and concentrating to obtain clear paste with the relative density of 1.15-1.25 at 60 ℃.
9. The preparation method of the plaster as claimed in claim 8, wherein the mass concentration of the ethanol solution is 60-70%, and the mass ratio of the traditional Chinese medicine powder to the ethanol solution is 1: 6-8 during reflux extraction.
10. The preparation method of the plaster according to the claim 7, wherein the mass concentration of the polydopamine modified metal organic framework material in the dispersion liquid in the step (2) is 10-15%, and the mass concentration of the sodium carboxymethylcellulose aqueous solution is 3-5%; the mass concentration of the gluconolactone solution is 10-20%.
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| CN114470508A (en) * | 2022-01-26 | 2022-05-13 | 中原工学院 | Physiotherapy salt pillow material with drug slow-release effect, preparation method and application |
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