CN115813773A - Traditional Chinese medicine mosquito-repellent water transfer printing air-sensitive reaction tattoo patch and preparation method thereof - Google Patents

Traditional Chinese medicine mosquito-repellent water transfer printing air-sensitive reaction tattoo patch and preparation method thereof Download PDF

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CN115813773A
CN115813773A CN202310007200.9A CN202310007200A CN115813773A CN 115813773 A CN115813773 A CN 115813773A CN 202310007200 A CN202310007200 A CN 202310007200A CN 115813773 A CN115813773 A CN 115813773A
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chinese medicine
mosquito
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CN115813773B (en
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王颖芳
田悦昕
陆滨欣
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Guangdong Pharmaceutical University
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Guangdong Pharmaceutical University
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    • Y02A50/00TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
    • Y02A50/30Against vector-borne diseases, e.g. mosquito-borne, fly-borne, tick-borne or waterborne diseases whose impact is exacerbated by climate change

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Abstract

The invention belongs to the technical field of stickers, and particularly relates to a traditional Chinese medicine mosquito-repellent water transfer printing air-sensitive reaction tattoo sticker and a preparation method thereof. The invention adopts a sonochemistry method to carry out nano microencapsulation on active volatile components of traditional Chinese medicinal materials, and then prepares the microencapsulated volatile extracted components of mosquito-repellent traditional Chinese medicines as functional layers into the mosquito-repellent water transfer printing gas-sensitive reaction tattoo patch. The mosquito repellent traditional Chinese medicine composition extract is used as a mosquito repellent, meets the requirement of people on pursuing safe natural plant component mosquito repellent, is natural, non-irritant, non-toxic or low-toxic, not easy to generate drug resistance, and has no pollution to the environment; nanometer microencapsulation is carried out on active ingredients of traditional Chinese medicinal materials, and the nanometer microencapsulation is combined with a gas-sensitive reaction tattoo patch technology, so that the tattoo patch which has a mosquito repelling effect and can be used for decorating a body is developed. In addition, the invention provides choices by utilizing the advantages of safe medicine, slow medicine release, convenient use, beautiful appearance and various styles, and is particularly suitable for children.

Description

Traditional Chinese medicine mosquito-repelling water transfer printing air-sensitive reaction tattooing paste and preparation method thereof
Technical Field
The invention belongs to the technical field of stickers, and particularly relates to a traditional Chinese medicine mosquito-repellent water transfer printing air-sensitive reaction tattoo sticker and a preparation method thereof.
Background
With the social development and the thought progress, the body of a young person is decorated or the personality of the young person is expressed in a tattooing mode, so that the young person can appeal to the fashion. Traditional tattooing techniques can be harmful: firstly, when a laser or operation method is adopted for making a tattoo or washing the tattoo, the skin is damaged, and wound infection may occur; secondly, the skin can not be restored to the original intact state after the traditional tattoo. The recent popular tattoo sticker makes up the defects of the traditional tattoo, is convenient to use, is noninvasive and painless, can change patterns at any time according to own favor, and is popular with young people. If the product has certain efficacy (such as mosquito repelling) while being attractive, the market prospect of the product is further expanded.
Mosquito repellent products on the market are abundant at present, and the first type is mosquito-repellent incense comprising traditional disc type mosquito-repellent incense, electric mosquito-repellent incense and liquid mosquito-repellent incense; the second is aerosol insecticides; the third category is repellents, such as essential balm, mosquito repellent toilet water, mosquito bite, etc.; the fourth category is electronic products, such as electric mosquito swatters, mosquito killing lamps, etc.; finally, mosquito nets and more new mosquito killing products with environmental protection, health and high-tech factors are provided. However, these mosquito repellent products have problems to be solved in different aspects and degrees in the using process. Consumers currently pay attention to the safety of products firstly when purchasing the products, and pay attention to the effect of the products secondly. Therefore, with the improvement of safety consciousness of people and the increasing fierce market competition, the relatively safe botanical mosquito-repellent itching-relieving products have wide market prospects.
In the prior art, there are many records about tattoo patches, for example, chinese patent ZL201910969207.2 discloses a water transfer tattoo sticker and a preparation and use method thereof, which discusses the preparation process of the water transfer tattoo patch in detail, the use method is simple, and the coloring dye is non-toxic and environment-friendly. But the tattoo paste is used as a tattoo paste, only plays a role of decoration, and has no related mosquito repelling function. Chinese patent ZL202010200331.5 discloses a gas-sensitive tattoo sticker, which is mainly attached on an object with its air inlet surface facing inwards, senses the taste of the object itself, and is used as a tool for disease monitoring, so that it can only be used as a tool, but has no related mosquito repelling function.
In conclusion, the technical problems that the tattoo is high in injury, cannot meet the requirements of all age groups of people, cannot meet the requirements of both decoration and functionality, is poor in mosquito repelling effect and the like generally exist in the prior art.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention aims to provide a traditional Chinese medicine mosquito-repellent water transfer printing air-sensitive reaction tattoo patch and a preparation method thereof. The traditional Chinese medicine mosquito-repellent water transfer printing air-sensitive reaction tattoo patch provided by the invention is provided with the air-sensitive reaction layer, and the nano microcapsules are used for wrapping the medicine, so that the tattoo patch reacts after contacting with the skin and slowly releases the medicine, thereby effectively ensuring the stability of the tattoo patch effect and prolonging the duration of mosquito-repellent effect.
In order to achieve the purpose, the technical scheme of the invention is as follows:
a preparation method of a traditional Chinese medicine mosquito-repellent water transfer printing air-sensitive reaction tattoo patch comprises the following steps:
s1, respectively performing microwave extraction on the traditional Chinese medicine components to obtain volatile components, and mixing the volatile components in proportion to obtain the volatile components of the traditional Chinese medicine;
s2, mixing the volatile components of the traditional Chinese medicinal materials prepared in the step S1 with mercapto chitosan, and then carrying out ultrasonic treatment to obtain a mixed solution of unreacted volatile components of the traditional Chinese medicines at the upper layer, microcapsule suspension liquid at the middle layer and unreacted mercapto chitosan at the lower layer;
s3, separating the mixed solution prepared in the step S2 by using a liquid transfer device to obtain a middle-layer microcapsule suspension, and freeze-drying to obtain microcapsule freeze-dried powder;
and S4, printing a design pattern on the surface of the polyvinyl alcohol film by using an ink jet printing transfer printing technology through genipin or genipin acid reagent, drying, mixing the microcapsule freeze-dried powder prepared in the step S3 and an adhesive in proportion, uniformly coating the mixture on the surface of the design pattern, drying in the air, and then attaching a protective film to the dried mixture to obtain the genipin or genipin acid microcapsule coating.
Further, the traditional Chinese medicine mosquito-repellent water transfer printing air-sensitive reaction tattoo patch is prepared by the method that in the step S1, the traditional Chinese medicine components comprise mint, mugwort, dried orange peel, folium artemisiae argyi, clove, verbena, rhizoma acori graminei, rosemary and basil, and the mass amount of each traditional Chinese medicine component is 30-50 parts.
Furthermore, in the preparation method of the traditional Chinese medicine mosquito repellent water transfer printing air-sensitive reaction tattoo patch, the mixing mass ratio of volatile components in the step S1 is mint: wild mugwort: dried orange peel: folium artemisiae argyi: clove: verbena: grassleaf sweelflag rhizome: rosemary: basil = 2.
Further, the preparation method of the traditional Chinese medicine mosquito repellent water transfer printing air-sensitive reaction tattoo patch comprises the following microwave extraction process in step S1: crushing the traditional Chinese medicine components (except dried orange peel, clove and verbena) according to the formula amount, sieving the crushed traditional Chinese medicine components with a 200-mesh sieve, adding an ethanol water solution with the volume of 6-10 times of that of the traditional Chinese medicine components, wherein the volume fraction of the ethanol water solution is 40-60%, soaking the traditional Chinese medicine components for 2h, performing microwave extraction, refluxing by adopting a spherical condensing tube, performing microwave extraction with the power of 400-500w for 10-20min, repeating the extraction for 3 times, filtering, combining the filtrate, and performing reduced pressure concentration on the filtrate to obtain the traditional Chinese medicine composition; the extraction solvent of the dried orange peel is water, the volume consumption of the water and the dried orange peel powder is 13-15, and the other extraction conditions are the same as the other traditional Chinese medicinal materials; the extraction solvent of the clove is petroleum ether, and the other extraction conditions are the same as those of other Chinese medicinal materials; the extraction solvent of the verbena is ethanol water solution with the volume fraction of 95%, the extraction power is 100w, and the other extraction conditions are the same as the other traditional Chinese medicine components.
Further, the preparation method of the traditional Chinese medicine mosquito repellent water transfer printing air-sensitive reaction tattoo patch comprises the following steps of: weighing 100mg of chitosan, dissolving the chitosan in an acetic acid solution with the volume fraction of 1% to prepare an acetic acid solution with the mass fraction of chitosan of 2.5%, then slowly dropwise adding a 5mol/L NaOH solution into the acetic acid solution, adjusting the pH value to 6.0, adding 13mg of 2-iminosulfane, stirring for about 12 hours, dialyzing the obtained solution in a 1mmol/L hydrochloric acid solution for 72 hours, intercepting the molecular weight of 7000Da, and then carrying out freeze drying treatment to obtain the chitosan.
Further, in the preparation method of the traditional Chinese medicine mosquito-repellent water transfer gas-sensitive reaction tattoo patch, the volatile components of the traditional Chinese medicine and the mercapto chitosan are mixed according to the volume ratio of 1:4-7 in the step S2.
Further, the preparation method of the traditional Chinese medicine mosquito repellent water transfer printing air-sensitive reaction tattoo patch comprises the following ultrasonic treatment process parameters in the step S2: the ultrasonic frequency is 70-100Hz, the ultrasonic time is 8-15min, and the ultrasonic temperature is 20-30 ℃.
Further, the preparation method of the traditional Chinese medicine mosquito repellent water transfer printing air-sensitive reaction tattoo patch comprises the following transfer printing conditions in step S4: the water temperature is 40-50 ℃, the relative humidity is 45-85%, and the drying temperature is 80-100 ℃.
Further, the preparation method of the traditional Chinese medicine mosquito repellent water transfer gas-sensitive reactive tattoo patch, in step S4, the preparation method of the genipin or genipin acid reagent is as follows: weighing 0.2g of genipin or geniposidic acid, and adding 15mL of ethanol for dissolving to obtain the genipin.
Further, in the preparation method of the traditional Chinese medicine mosquito-repellent water transfer gas-sensitive reactive tattoo patch, in the step S4, the drying temperature is less than or equal to 40 ℃, and the mixing ratio of the microcapsule suspension freeze-dried powder and the adhesive is 1:1.
Further, in the preparation method of the traditional Chinese medicine mosquito repellent water transfer gas-sensitive reactive tattoo patch, in the step S4, the adhesive is polymethyl methacrylate.
The invention also provides the traditional Chinese medicine mosquito repelling water transfer gas sensitive reaction tattoo patch prepared by the preparation method of the traditional Chinese medicine mosquito repelling water transfer gas sensitive reaction tattoo patch.
The mint in the traditional Chinese medicine components is fragrant and disperse, and the smashed mint leaves are applied to mosquito bites, so that the itching relieving effect is good; mugwort has strong peculiar smell; the dried orange peel contains linalool which has toxicity, oviposition deterrence and repellency to a plurality of insects. The folium artemisiae argyi can dispel mosquitoes, and is smoked in the house for Ai Keda to achieve the aim of repelling mosquitoes. The eugenol extracted from clove is used for preparing mosquito repellent liquid, and is nontoxic and harmless to human body. The volatile components of verbena have strong antibacterial effect. The grassleaf sweelflag rhizome has aromatic smell, can repel dirt and eliminate turbid, has the efficacy of detoxifying and eliminating evil and can repel mosquitoes; rosemary has bacteriostatic properties. Basil has pleasant fragrance and strong mosquito repelling effect. The compatibility of the medicines can play the roles of fragrance, dirt avoidance and mosquito repelling.
The natural plant traditional Chinese medicine components with the mosquito repelling effect are selected to extract volatile components to prepare the mosquito repelling tattoo patch, the components have obvious mosquito repelling effect, have toxic killing, avoiding, food refusing and growth inhibiting effects on insects, contain plant source active components with insect sex pheromone attracting effect, have fragrant smell, are easy to volatilize, have high biological activity on mosquitoes, have low toxicity to people and mammals, have no residue, have no pollution to the environment, and improve the product safety to a great extent. Meanwhile, the insecticidal composition has the antibacterial and anti-inflammatory effects, and can effectively prevent and treat the infection of mosquitoes, flies, lice and other sanitary pests on human bodies.
According to the invention, after the volatile components of the traditional Chinese medicinal materials and the mercapto chitosan are mixed, ultrasonic treatment can be carried out to ensure that the mercapto chitosan and the volatile components of the traditional Chinese medicinal materials can better form microcapsules, the ultrasonic treatment time can influence the particle size and the subsequent slow release time of the formed microcapsules, the ultrasonic reaction time is too long, and the optimal structural state of the microcapsules can be damaged, so that the action time of the volatile components of the traditional Chinese medicinal materials is influenced, the mosquito repellent effect is reduced, and meanwhile, the particle size of the microcapsules can be reduced and the wrapping amount of the volatile components of the traditional Chinese medicinal materials is reduced due to the too long ultrasonic time; the ultrasonic reaction time is too short, the volatile components of the traditional Chinese medicine are not completely wrapped by the sulfhydryl chitosan, and complete microcapsules cannot be formed, so that the action time of the volatile components of the traditional Chinese medicine is shortened, and the mosquito repelling effect is reduced. In addition, the invention adopts a sonochemistry method to microencapsulate the volatile components of the mosquito-repellent traditional Chinese medicine, active sulfhydryl groups are induced to crosslink through ultrasonic treatment to generate disulfide bonds, and the natural high molecular material containing the active sulfhydryl groups can crosslink through the cavitation effect of sonochemistry and deposit on the surfaces of oil drops dispersed by the ultrasonic emulsification to form the microcapsules.
The invention adopts the nanometer microcapsule wrapping technology to realize the slow release effect, the microencapsulation can change the physical and chemical properties of the core material such as color, shape, volume, density, stability and the like, and simultaneously, the core material is separated from the external environment, thereby avoiding the direct contact of the core material and the external environment, protecting the core material from being interfered by the external environment and releasing the core material only when needed. Volatile components of the mosquito-repellent traditional Chinese medicine are extracted by a microwave extraction method, and the microencapsulated mosquito-repellent traditional Chinese medicine is added to a tattoo patch reaction layer, so that the skin is not directly contacted, the discomfort of the skin is relieved, the transdermal absorption speed is slowed, and the drug effect is prolonged.
The active ingredients are wrapped by selecting sulfydryl chitosan as a capsule wall material, and the chitosan serving as a natural high polymer has good film-forming property and antibacterial property and a plurality of unique physicochemical characteristics and biological functions, but has poor solubility and insufficient antibacterial activity due to hydrogen bonds between molecules and in molecules of the chitosan. Therefore, the invention utilizes free amino and hydroxyl in chitosan molecules to carry out chemical reaction to carry out chemical modification on chitosan. The obtained derivative has good film forming property, hygroscopicity, adhesion and biodegradability. The thiolated chitosan not only has the excellent properties of chitosan, but also has good water solubility, improves the limit of water insolubility of the chitosan, has strong adhesion and no biotoxicity, and is particularly suitable for wrapping the active ingredients of the mosquito-repellent traditional Chinese medicine. In addition, the chitosan has rich sources, is non-toxic and biodegradable, is a green, environment-friendly and environment-friendly material, and accords with the environment-friendly and safe product pursued by the public at present.
Compared with the prior art, the preparation method of the traditional Chinese medicine mosquito-repellent water transfer printing air-sensitive reaction tattoo patch provided by the invention has the following technical advantages:
(1) According to the invention, the water transfer printing paper adopts the strippable water mark transfer printing paper, and a layer of protective gloss oil is formed on the surface of the water transfer printing paper during generation, so that protective paint does not need to be coated;
(2) The mosquito repellent traditional Chinese medicine composition extract is used as a mosquito repellent, meets the requirement of people on pursuing safe natural plant component mosquito repellent, is natural, non-irritant, non-toxic or low-toxic, not easy to generate drug resistance, and has no pollution to the environment;
(3) The invention combines the microencapsulation technology, uses the effective components of the aromatic mosquito-repellent traditional Chinese medicine which are screened and extracted in the early stage, carries out nano microencapsulation on, combines the technology with the gas-sensitive reaction tattoo paste technology, develops the tattoo paste which has the mosquito-repellent effect and can be used for decorating the body;
(4) The invention provides choices by utilizing the advantages of safe medicine, slow medicine release, convenient use, beautiful appearance and various styles, and is particularly suitable for children.
Detailed Description
The present invention is further described below by way of specific embodiments, but the present invention is not limited to only the following examples. Various modifications may be made by those skilled in the art based on the basic idea of the invention, but it is within the scope of the invention as long as it does not depart from the basic idea of the invention.
In this embodiment, the preparation method of the traditional Chinese medicine mosquito-repellent water transfer gas-sensitive reaction tattoo patch, in step S2, comprises the following steps: weighing 100mg of chitosan, dissolving the chitosan in an acetic acid solution with the volume fraction of 1% to prepare an acetic acid solution with the mass fraction of chitosan of 2.5%, then slowly dropwise adding a 5mol/L NaOH solution into the acetic acid solution, adjusting the pH value to 6.0, adding 13mg of 2-iminosulfane, stirring for about 12 hours, dialyzing the obtained solution in a 1mmol/L hydrochloric acid solution for 72 hours, intercepting the molecular weight of 7000Da, and then carrying out freeze drying treatment to obtain the chitosan. The preparation method of the genipin or the genipin nucleotide reagent in the step S4 comprises the following steps: weighing 0.2g of genipin or geniposidic acid, and adding 15mL of ethanol for dissolving to obtain the genipin. In the step S4, the drying temperature is less than or equal to 40 ℃, and the mixing ratio of the microcapsule suspension freeze-dried powder to the adhesive is 1:1. In the step S4, the adhesive is polymethyl methacrylate.
Example 1 preparation method of traditional Chinese medicine mosquito-repellent water transfer printing air-sensitive reaction tattoo patch
The preparation method of the traditional Chinese medicine mosquito-repellent water transfer printing air-sensitive reaction tattoo patch comprises the following steps:
s1, respectively performing microwave extraction on the traditional Chinese medicine components to obtain volatile components, and mixing the volatile components in proportion to obtain the volatile components of the traditional Chinese medicine;
s2, mixing the volatile components of the traditional Chinese medicinal materials prepared in the step S1 with mercapto chitosan, and then carrying out ultrasonic treatment to obtain a mixed solution of unreacted volatile components of the traditional Chinese medicines at the upper layer, microcapsule suspension liquid at the middle layer and unreacted mercapto chitosan at the lower layer;
s3, separating the mixed solution prepared in the step S2 by using a liquid transfer device to obtain a middle-layer microcapsule suspension, and freeze-drying to prepare microcapsule freeze-dried powder;
and S4, printing a designed pattern on the surface of the polyvinyl alcohol film by using an ink-jet printing technology, drying, mixing the microcapsule freeze-dried powder prepared in the step S3 and an adhesive in proportion, uniformly coating the mixture on the surface of the designed pattern, drying, and attaching a protective film to the dried mixture to obtain the product.
The traditional Chinese medicine components in the step S1 are mint, wild artemisia, dried orange peel, folium artemisiae argyi, clove, verbena, rhizoma acori graminei, rosemary and basil, and the dosage of each traditional Chinese medicine component is 30 parts; the mixing proportion of the volatile components is as follows: wild mugwort: dried orange peel: folium artemisiae argyi: clove: verbena: grassleaved sweetflag: rosemary: 2. The microwave extraction process comprises the following steps: the preparation method of the traditional Chinese medicine mosquito-repellent water transfer printing air-sensitive reaction tattoo patch comprises the following microwave extraction process in step S1: crushing the traditional Chinese medicine components (except dried orange peel, clove and verbena) according to the formula amount, sieving the crushed traditional Chinese medicine components with a 200-mesh sieve, adding an ethanol water solution with the volume of 6 times of that of the traditional Chinese medicine components, wherein the volume fraction of the ethanol water solution is 40%, soaking the traditional Chinese medicine components for 2h, performing microwave extraction, refluxing by adopting a spherical condenser tube, performing microwave extraction with the power of 400w for 10min, repeating extraction for 3 times, filtering, combining filtrates, and concentrating the filtrate under reduced pressure to obtain the traditional Chinese medicine composition; the extraction solvent of the dried orange peel is water, the volume consumption of the water and the dried orange peel powder is 13, and the other extraction conditions are the same as the other traditional Chinese medicinal materials; the extraction solvent of the clove is petroleum ether, and the other extraction conditions are the same as those of other Chinese medicinal materials; the extraction solvent of the verbena is ethanol water solution with the volume fraction of 95%, the extraction power is 100w, and the other extraction conditions are the same as the other traditional Chinese medicine components.
Mixing the volatile components of the traditional Chinese medicinal materials and the mercapto chitosan according to a volume ratio of 1:4 in the step S2; the ultrasonic treatment process parameters are as follows: the ultrasonic frequency is 70Hz, the ultrasonic time is 15min, and the ultrasonic temperature is 20 ℃.
The transfer conditions in step S4 are: the water temperature is 40 ℃, the relative humidity is 45%, and the drying temperature is 80 ℃.
Embodiment 2, preparation method of traditional Chinese medicine mosquito-repellent water transfer printing air-sensitive reaction tattoo patch
The preparation method of the traditional Chinese medicine mosquito-repellent water transfer printing air-sensitive reaction tattoo patch comprises the following steps:
s1, respectively performing microwave extraction on the traditional Chinese medicine components to obtain volatile components, and mixing the volatile components in proportion to obtain the volatile components of the traditional Chinese medicine;
s2, mixing the volatile components of the traditional Chinese medicinal materials prepared in the step S1 with mercapto chitosan, and then carrying out ultrasonic treatment to obtain a mixed solution of unreacted volatile components of the traditional Chinese medicines at the upper layer, microcapsule suspension liquid at the middle layer and unreacted mercapto chitosan at the lower layer;
s3, separating the mixed solution prepared in the step S2 by using a liquid transfer device to obtain a middle-layer microcapsule suspension, and freeze-drying to obtain microcapsule freeze-dried powder;
and S4, printing a designed pattern on the surface of the polyvinyl alcohol film by using an ink-jet printing technology, drying, mixing the microcapsule freeze-dried powder prepared in the step S3 and an adhesive in proportion, uniformly coating the mixture on the surface of the designed pattern, drying, and attaching a protective film to the dried mixture to obtain the product.
The traditional Chinese medicine components in the step S1 are mint, mugwort, dried orange peel, folium artemisiae argyi, clove, verbena, rhizoma acori graminei, rosemary and basil, and the dosage of each traditional Chinese medicine component is 50 parts; the mixing proportion of the volatile components is as follows: wild mugwort: dried orange peel: folium artemisiae argyi: clove: verbena: grassleaf sweelflag rhizome: rosemary: 2. The microwave extraction process comprises the following steps: the preparation method of the traditional Chinese medicine mosquito-repellent water transfer printing air-sensitive reaction tattoo patch comprises the following microwave extraction process in step S1: crushing the traditional Chinese medicine components (except dried orange peel, clove and verbena) according to the formula amount, sieving the crushed traditional Chinese medicine components with a 200-mesh sieve, adding an ethanol water solution with the volume 10 times of that of the traditional Chinese medicine components, soaking the ethanol water solution for 2h, performing microwave extraction, refluxing by adopting a spherical condenser tube, wherein the microwave extraction power is 500w, the extraction time is 20min, repeating the extraction for 3 times, filtering, combining the filtrates, and concentrating the filtrate under reduced pressure to obtain the traditional Chinese medicine composition; the extraction solvent of the dried orange peel is water, the volume consumption of the water and the dried orange peel powder is 15, and the other extraction conditions are the same as the other traditional Chinese medicinal materials; the extracting solvent of the clove is petroleum ether, and the other extracting conditions are the same as those of other traditional Chinese medicine components; the extraction solvent of the verbena is ethanol water solution with the volume fraction of 95%, the extraction power is 100w, and the other extraction conditions are the same as the other traditional Chinese medicine components.
Mixing the volatile components of the traditional Chinese medicinal materials and the mercapto chitosan according to a volume ratio of 1:7 in the step S2; the ultrasonic treatment process parameters are as follows: the ultrasonic frequency is 100Hz, the ultrasonic time is 8min, and the ultrasonic temperature is 30 ℃.
The transfer conditions in step S4 are: the water temperature is 50 ℃, the relative humidity is 85%, and the drying temperature is 100 ℃.
Example 3 preparation method of traditional Chinese medicine mosquito-repellent water transfer printing air-sensitive reaction tattoo patch
The preparation method of the traditional Chinese medicine mosquito-repellent water transfer printing air-sensitive reaction tattoo patch comprises the following steps:
s1, respectively performing microwave extraction on the traditional Chinese medicine components to obtain volatile components, and mixing the volatile components in proportion to obtain the volatile components of the traditional Chinese medicine;
s2, mixing the volatile components of the traditional Chinese medicinal materials prepared in the step S1 with mercapto chitosan, and then carrying out ultrasonic treatment to obtain a mixed solution of unreacted volatile components of the traditional Chinese medicines at the upper layer, microcapsule suspension liquid at the middle layer and unreacted mercapto chitosan at the lower layer;
s3, separating the mixed solution prepared in the step S2 by using a liquid transfer device to obtain a middle-layer microcapsule suspension, and freeze-drying to obtain microcapsule freeze-dried powder;
and S4, printing a designed pattern on the surface of the polyvinyl alcohol film by using an ink-jet printing technology, drying, mixing the microcapsule freeze-dried powder prepared in the step S3 and an adhesive in proportion, uniformly coating the mixture on the surface of the designed pattern, drying, and attaching a protective film to the dried mixture to obtain the product.
The traditional Chinese medicine components in the step S1 are mint, wild artemisia, dried orange peel, folium artemisiae argyi, clove, verbena, rhizoma acori graminei, rosemary and basil, and the dosage of each traditional Chinese medicine component is 40 parts; the mixing proportion of the volatile components is as follows: wild mugwort: dried orange peel: folium artemisiae argyi: clove: verbena: grassleaf sweelflag rhizome: rosemary: 2. The microwave extraction process comprises the following steps: the preparation method of the traditional Chinese medicine mosquito-repellent water transfer printing air-sensitive reaction tattoo patch comprises the following microwave extraction process in step S1: crushing the traditional Chinese medicine components (except dried orange peel, clove and verbena) according to the formula amount, sieving the crushed traditional Chinese medicine components with a 200-mesh sieve, adding an ethanol water solution with the volume of 8 times of that of the traditional Chinese medicine components, wherein the volume fraction of the ethanol water solution is 50%, soaking the traditional Chinese medicine components for 2h, performing microwave extraction, refluxing by adopting a spherical condenser tube, performing microwave extraction with the power of 450w for 16min, repeating extraction for 3 times, filtering, combining filtrates, and concentrating the filtrate under reduced pressure to obtain the traditional Chinese medicine composition; the extraction solvent of the dried orange peel is water, the volume consumption of the water and the dried orange peel powder is 14, and the other extraction conditions are the same as the other traditional Chinese medicinal materials; the extracting solvent of the clove is petroleum ether, and the other extracting conditions are the same as those of other traditional Chinese medicine components; the extraction solvent of the verbena is ethanol water solution with the volume fraction of 95%, the extraction power is 100w, and the other extraction conditions are the same as the other traditional Chinese medicine components.
Mixing the volatile components of the traditional Chinese medicinal materials in the step S2 with mercapto chitosan according to a volume ratio of 1:6; the ultrasonic treatment process parameters are as follows: the ultrasonic frequency is 85Hz, the ultrasonic time is 10min, and the ultrasonic temperature is 25 ℃.
The transfer conditions in step S4 are: the water temperature is 45 ℃, the relative humidity is 60%, and the drying temperature is 90 ℃.
Comparative example 1 preparation method of traditional Chinese medicine mosquito-repellent water transfer printing air-sensitive reaction tattooing patch
The preparation method of the traditional Chinese medicine mosquito-repellent water transfer gas-sensitive reaction tattoo patch in the comparative example is similar to that in example 3.
The comparative example differs from example 3 in that: in the comparative example, the volatile components of the traditional Chinese medicinal materials in the step S2 are mixed with the mercapto chitosan according to the volume ratio of 1:1.
Comparative example 2 preparation method of traditional Chinese medicine mosquito-repellent water transfer printing air-sensitive reaction tattoo patch
The preparation method of the traditional Chinese medicine mosquito-repellent water transfer gas-sensitive reaction tattoo patch in the comparative example is similar to that in example 3.
The comparative example differs from example 3 in that: in this comparative example carboxymethyl cellulose was used instead of mercaptochitosan.
Comparative example 3 preparation method of traditional Chinese medicine mosquito-repellent water transfer printing air-sensitive reaction tattooing patch
The preparation method of the traditional Chinese medicine mosquito repellent water transfer gas-sensitive reaction tattooing patch in the comparative example is similar to that in example 3.
The difference between this comparative example and example 3 is: the ultrasonic frequency in step S2 described in this comparative example was 180Hz.
Comparative example 4 preparation method of traditional Chinese medicine mosquito-repellent water transfer printing air-sensitive reaction tattoo patch
The preparation method of the traditional Chinese medicine mosquito repellent water transfer gas-sensitive reaction tattooing patch in the comparative example is similar to that in example 3.
The difference between this comparative example and example 3 is: the ultrasonic frequency in step S2 described in this comparative example was 20Hz.
Comparative example 5 preparation method of traditional Chinese medicine mosquito-repellent water transfer printing air-sensitive reaction tattoo patch
The preparation method of the traditional Chinese medicine mosquito-repellent water transfer gas-sensitive reaction tattoo patch in the comparative example is similar to that in example 3.
The difference between this comparative example and example 3 is: the sonication time in step S2 described in this comparative example was 30min.
Comparative example 6 preparation method of traditional Chinese medicine mosquito-repellent water transfer printing air-sensitive reaction tattooing patch
The preparation method of the traditional Chinese medicine mosquito-repellent water transfer gas-sensitive reaction tattoo patch in the comparative example is similar to that in example 3.
The difference between this comparative example and example 3 is: the sonication time in step S2 described in this comparative example was 2min.
Test example, mosquito repellent Effect test
Test samples: the important mosquito repellent water transfer printing air-sensitive reaction tattoo patches prepared in the examples 1-3 and the comparative examples 1-6; control group: adopting clear water to replace volatile components of the traditional Chinese medicinal materials to prepare the tattoo patch;
the test method comprises the following steps: the prepared mosquito repelling nano microcapsule mosquito repelling water transfer printing air-sensitive reaction tattoo sticker is used for mosquito repelling detection by using a Y-type olfactometer, the angles of two arms of the Y-type tube are adjusted, and the air speed is provided by a vacuum pump, so that experimental data errors caused by the fact that other external factors influence mosquito tendency are avoided. And according to the adjusted angle and wind speed, the wind speed is used for the next detection. Sample is putThe test group and the control group are respectively marked at one end of the sample chamber. And (4) placing mosquitoes, starting the device for 30s, recording results, and recording the number of the two-armed mosquitoes at 1 min, 2min, 4 min, 6min, 8min and 10min respectively. Each group was repeated 5-8 times, the average value was recorded, and the avoidance rate at 10min, the avoidance rate (effective protection rate)% = (N) 1 -N 2 )/(N 1 +N 2 );N 1 : represents the number of the control group of the pipe wall mosquitoes; n is a radical of 2 : the number of mosquitoes in the tube wall of the test group is shown.
And (3) test results: the test results are shown in Table 1.
TABLE 1 mosquito repelling effect test results
Figure 964703DEST_PATH_IMAGE001
As can be seen from table 1, the traditional Chinese medicine mosquito repelling water transfer printing air-sensitive reactive tattoo patch prepared by the invention has a good mosquito repelling effect, the mosquito repelling rate of 10min is more than 85%, wherein the traditional Chinese medicine mosquito repelling water transfer printing air-sensitive reactive tattoo patch prepared in example 3 has the highest repelling rate, and is the best embodiment of the invention.
Compared with the embodiment 3, the proportion of the volatile components of the traditional Chinese medicinal materials to the mercapto chitosan is changed in the comparative example 1, but the mosquito repellent effect of the prepared tattoo patch is poor, and the avoidance rate of 10min is reduced to 72.1%, because the proportion of the volatile components of the traditional Chinese medicinal materials to the mercapto chitosan is changed, the volatile components of the traditional Chinese medicinal materials are not completely wrapped by the mercapto chitosan, and the mosquito repellent effect is poor; comparative example 2 adopts common microcapsule wall material carboxymethyl cellulose to replace sulfhydryl chitosan, but the mosquito repellent effect of the prepared tattoo patch is poor, which shows that not all microcapsule wall materials can realize the technical effect of sulfhydryl chitosan of the invention.
Compared example 3, the ultrasonic frequency is increased, the ultrasonic time is prolonged in compared example 5, but the mosquito repellent effect of the prepared tattoo patch is poor, and the avoidance rate is reduced, because the optimal structural state of the microcapsule is destroyed due to overhigh ultrasonic frequency or overlong ultrasonic time, so that the action time of the volatile components of the traditional Chinese medicinal materials is influenced, the mosquito repellent effect is reduced, and meanwhile, the particle size of the microcapsule is reduced due to overlong ultrasonic time, and the wrapping amount of the volatile components of the traditional Chinese medicinal materials is reduced; compared example 4, the ultrasonic frequency is reduced, and the ultrasonic time is shortened in compared example 6, but the mosquito repellent effect of the prepared tattoo patch is poor, and the avoidance rate is reduced, because the ultrasonic reaction time is too short or the ultrasonic frequency is too low, the mercapto chitosan does not completely wrap the volatile components of the traditional Chinese medicine, and can not form complete microcapsules, so that the action time of the volatile components of the traditional Chinese medicine is shortened, and the mosquito repellent effect is reduced.
The above examples are merely illustrative of the preparation process of the present invention and are not intended to be limiting. Those skilled in the art should not be able to modify the above embodiments without departing from the spirit and scope of the present invention. Accordingly, it is intended that all equivalent modifications or changes which can be made by those skilled in the art without departing from the technical spirit of the present invention are covered by the claims of the present invention.

Claims (10)

1. A preparation method of a traditional Chinese medicine mosquito-repellent water transfer printing air-sensitive reaction tattoo patch is characterized by comprising the following steps:
s1, respectively performing microwave extraction on the traditional Chinese medicine components to obtain volatile components, and mixing the volatile components in proportion to obtain the volatile components of the traditional Chinese medicine;
s2, mixing the volatile components of the traditional Chinese medicinal materials prepared in the step S1 with mercapto chitosan, and then carrying out ultrasonic treatment to obtain a mixed solution of unreacted volatile components of the traditional Chinese medicines at the upper layer, microcapsule suspension liquid at the middle layer and unreacted mercapto chitosan at the lower layer;
s3, separating the mixed solution prepared in the step S2 by using a liquid transfer device to obtain a middle-layer microcapsule suspension, and freeze-drying to obtain microcapsule freeze-dried powder;
and S4, printing a design pattern on the surface of the polyvinyl alcohol film by using an ink jet printing transfer printing technology through genipin or genipin acid reagent, drying, mixing the microcapsule freeze-dried powder prepared in the step S3 and an adhesive in proportion, uniformly coating the mixture on the surface of the design pattern, drying in the air, and then attaching a protective film to the dried mixture to obtain the genipin or genipin acid microcapsule coating.
2. The preparation method of the traditional Chinese medicine mosquito-repelling water transfer gas-sensitive reaction tattooing patch according to claim 1, wherein the traditional Chinese medicine components in the step S1 are mint, mugwort, dried orange peel, mugwort leaf, clove, verbena, grassleaf sweelflag rhizome, rosemary and basil, and the mass amount of each traditional Chinese medicine component is 30-50 parts.
3. The preparation method of the traditional Chinese medicine mosquito-repelling water transfer gas-sensitive reaction tattooing patch according to claim 1, wherein the mixing mass ratio of volatile components in the step S1 is mint: wild mugwort: dried orange peel: folium artemisiae argyi: clove: verbena: grassleaf sweelflag rhizome: rosemary: 2.
4. The preparation method of the traditional Chinese medicine mosquito-repelling water transfer gas-sensitive reaction tattoo patch according to claim 2, wherein the microwave extraction process in the step S1 is as follows: the preparation method of the traditional Chinese medicine mosquito-repellent water transfer printing air-sensitive reaction tattoo patch comprises the following microwave extraction process in step S1: crushing the traditional Chinese medicine components except the dried orange peel, the clove and the verbena, sieving the crushed traditional Chinese medicine components with a 200-mesh sieve, adding an ethanol water solution with the volume of 6-10 times of that of the traditional Chinese medicine components, wherein the volume fraction of the ethanol water solution is 40-60%, soaking for 2h, performing microwave extraction, refluxing by adopting a spherical condensing tube, performing microwave extraction with the power of 400-500w for 10-20min, repeating the extraction for 3 times, filtering, combining the filtrate, and performing reduced pressure concentration on the filtrate to obtain the traditional Chinese medicine composition; the extraction solvent of the dried orange peel is water, and the volume consumption of the water and the dried orange peel powder is 13-15; the extraction solvent of the clove is petroleum ether; the extraction solvent of the verbena is ethanol water solution with the volume fraction of 95%, and the extraction power is 100w.
5. The preparation method of the traditional Chinese medicine mosquito-repelling water transfer printing gas-sensitive reaction tattooing patch according to claim 1, wherein the preparation method of the sulfhydryl chitosan in the step S2 is as follows: weighing 100mg of chitosan, dissolving the chitosan in an acetic acid solution with the volume fraction of 1% to prepare an acetic acid solution with the mass fraction of chitosan of 2.5%, then slowly dropwise adding a 5mol/L NaOH solution into the acetic acid solution, adjusting the pH value to 6.0, adding 13mg of 2-iminosulfane, stirring for 12 hours, dialyzing the obtained solution in a 1mmol/L hydrochloric acid solution for 72 hours, intercepting the molecular weight of 7000Da, and then carrying out freeze drying treatment to obtain the chitosan-based aqueous solution.
6. The preparation method of the traditional Chinese medicine mosquito-repellent water transfer gas-sensitive reaction tattooing patch according to claim 1, wherein in the step S2, the volatile components of the traditional Chinese medicine are mixed with mercapto chitosan according to a volume ratio of 1:4-7; the ultrasonic treatment process parameters in the step S2 are as follows: the ultrasonic frequency is 70-100Hz, the ultrasonic time is 8-15min, and the ultrasonic temperature is 20-30 ℃.
7. The preparation method of the traditional Chinese medicine mosquito-repellent water transfer gas-sensitive reactive tattoo patch according to claim 1, wherein the transfer conditions in step S4 are as follows: the water temperature is 40-50 ℃, the relative humidity is 45-85%, and the drying temperature is 80-100 ℃.
8. The preparation method of the traditional Chinese medicine mosquito-repelling water transfer printing air-sensitive reaction tattooing patch according to claim 1, wherein the preparation method of the genipin or genipin acid reagent in the step S4 is as follows: weighing 0.2g of genipin or geniposidic acid, and adding 15mL of ethanol for dissolving to obtain the genipin.
9. The preparation method of the traditional Chinese medicine mosquito-repellent water transfer gas-sensitive reaction tattoo patch according to claim 1, wherein the drying temperature in the step S4 is less than or equal to 40 ℃; the mixing mass ratio of the microcapsule suspension freeze-dried powder to the adhesive is 1:1; the adhesive is polymethyl methacrylate.
10. A traditional Chinese medicine mosquito repellent water transfer gas sensitive reaction tattoo patch prepared by the preparation method of the traditional Chinese medicine mosquito repellent water transfer gas sensitive reaction tattoo patch according to any one of claims 1-9.
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