CN109045069B - Earthworm syrup nano-silver hydrogel patch and preparation method thereof - Google Patents

Earthworm syrup nano-silver hydrogel patch and preparation method thereof Download PDF

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CN109045069B
CN109045069B CN201811328175.XA CN201811328175A CN109045069B CN 109045069 B CN109045069 B CN 109045069B CN 201811328175 A CN201811328175 A CN 201811328175A CN 109045069 B CN109045069 B CN 109045069B
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李丽霞
卢先云
李芳龙
冯鑫
陈容
殷中琼
邹元锋
宋旭
梁晓霞
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Sichuan Agricultural University
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Abstract

The invention discloses a earthworm syrup nano-silver hydrogel patch and a preparation method thereof, wherein the preparation method comprises the steps of preparing earthworm syrup; preparing nano silver sol; preparing the earthworm syrup nano-silver hydrogel patch. The patch is prepared by adding the antibacterial material nano-silver into the earthworm syrup, and has strong combination, so that the earthworm syrup is efficient and safe and is not easy to generate drug resistance; the prepared hydrogel patch has the advantages of convenience, comfort, no pollution to clothes, high drug utilization rate, continuous cooling effect, contribution to wound healing, and improvement on drug effect and quality of products.

Description

Earthworm syrup nano-silver hydrogel patch and preparation method thereof
Technical Field
The invention belongs to the technical field of drug research and development, and particularly relates to a earthworm syrup nano-silver hydrogel patch and a preparation method thereof.
Background
Burn and scald are the common accidental injuries in daily life, and cause of the burn and scald are different, but the primary principles for treating the burn and scald are all consistent, and the problems of infection, pain, healing and the like of a wound surface generally need to be solved by clearing heat. At present, a plurality of burn and scald medicines mainly comprise two aspects of traditional Chinese medicines and western medicines, the traditional Chinese medicines have slow effect and are relatively complex to prepare, and the western medicines have quick drug effect but are easy to generate drug resistance; the dosage forms are mostly ointment, oil and the like, which easily pollute clothes and are inconvenient to use.
The earthworm is a dried body of a lumbricus king or onymus tricolor of lumbridae, and is recorded in the monograph of medical monographs of the past generation of the poetry of the peripheral generation, and also named as earthworm, ricefield eel, jianwei, earthworm and the like. Earthworm is salty and cold in nature, has the efficacies of clearing heat, arresting convulsion, relieving asthma, dredging collaterals and promoting blood circulation, and is recorded in compendium of materia medica: the earthworm can treat ulcerated oral aphthae and tongue aphthae, and is clinically used for treating various diseases such as burns, scalds and lower limb ulceration. According to modern pharmacological research, the earthworm has the effects of reducing blood pressure, resisting thrombus, dissolving thrombus, improving blood circulation, relieving asthma, resisting arrhythmia, relieving fever, resisting inflammation, relieving pain, accelerating wound healing and the like. In recent years, a plurality of Chinese and foreign students research the effects of earthworm on wound healing, and the research finds that the earthworm contains various active ingredients such as earthworm extract, earthworm alkali, amino acid, alkaloid, linoleic acid, peptide, zinc and the like, has the effects of detoxifying, promoting blood circulation to remove blood stasis, resisting inflammation and resisting infection obviously, can promote the hyperplasia of capillary vessels, fibroblasts and myofibroblasts, and can accelerate the tissue repair process of wound surfaces. Studies by Zhongying et al indicate that: the earthworm protein promotes rat fibroblast (NIH) at molecular level3T3) Proliferation and collagen synthesis, thereby promoting the healing of rat deep II degree scald macroscopically (Zhongying, xi, Song Shuliang, etc.. earthworm protein has healing promoting effect on rat deep II degree scald [ J]China journal of trauma, 2010,26(4): 377-379.).
Earthworm syrup is a folk prescription with a long history and can be used for treating various skin diseases such as epidemic parotitis, herpes zoster, ulcer of lower limbs, erysipelas, burn and scald, and the like. The preparation method comprises cleaning fresh Lumbricus, adding appropriate amount of white sugar, continuously exuding Lumbricus body fluid, and gradually shrinking to obtain light yellow leachate, which is Lumbricus syrup. The folk prescription has obvious effect in folk medicine application and very wide application, and people begin to use the earthworm syrup to treat burns and scalds as early as 70 years, and obtains more satisfactory curative effect. The earthworm is leached by white sugar, the white sugar is cool in nature, the white sugar infusion is a hypertonic solution and has the functions of absorbing water and preventing corrosion, and the earthworm is cold in nature and can clear heat, heal wound, promote blood circulation and remove meridian obstruction. The combination of the two can not only clear away heat and toxic materials, heal wound and promote granulation, but also protect pain nerve endings, play the efficacy of promoting blood circulation and removing blood stasis and have obvious analgesic effect; and the effects of promoting wound healing, resisting infection and the like, so the Chinese medicinal composition has good treatment effect on burns and scalds. According to research, the earthworm syrup is used for treating the burn and scald, the wound surface has no pain, exudation and infection, the original infected wound surface can be quickly controlled, the burn and scald wound surface within II degrees can be healed within 2 weeks, few scars are left after healing, the shallow III degree burn and scald wound surface can be healed within 3 weeks, slight scars are left, no scar is found, and the cure rate is 100%.
Silver is used as the most commonly used antibacterial agent, has the advantages of high efficiency, broad spectrum, safety and the like, and is widely applied to antibacterial and mildew-proof products, while nano-silver is used as a novel polymer material in the 21 st century, has wide application prospects in the fields of antibacterial, catalysis, lubricants, optics, electric conduction, biological materials and the like, and is one of the research hotspots in the medical field due to the advantages of high safety, high efficiency, broad spectrum, difficult generation of drug resistance and the like of nano-silver. The nano-silver burn patch is applied to treat small-area burn in the early years of the burn department in the morning light hospital, Fushun county, Fushun, Sichuan province, and has excellent treatment effect and higher safety. The nano silver dressing is mainly compounded with other substances in the aspect of treating burns and scalds, such as moist burn ointment (MEBO), so that the nano silver dressing can prevent and treat infection, accelerate wound healing and effectively relieve later-stage scar contracture. The nano-silver medical antibacterial dressing is matched with reasonable and correct treatment and nursing, so that the cure rate can be improved, the regeneration and repair of the wound surface can be promoted, and the generation of scars can be reduced and avoided; in addition, the nano-silver gel is also frequently applied clinically, and has double effects of resisting infection and promoting healing of infectious wound surfaces, so that the nano-silver gel is particularly advantageous in the aspect of treating burns and scalds.
A hydrogel patch, also called cataplasm, is an external patch prepared by taking a water-soluble polymer material as a main matrix, adding a medicament and coating the mixture on non-woven fabrics, and belongs to a dosage form of a transdermal drug delivery system; first in japan in the seventies. Compared with other medicine preparations, the preparation has the advantages of large drug-loading rate, accurate dosage, good application property and moisture retention property, no sensitization and irritation, convenient and comfortable use, no pollution to clothes, no adverse reaction such as lead poisoning and the like. Thus, hydrogel patches are considered to be a new formulation with great market potential. Moreover, the hydrogel patch has been found to enhance transdermal penetration of proteins without affecting the activity of the proteins. The basic composition of a hydrogel patch matrix generally includes a cross-linked backbone, a cross-linking agent, a cross-linking modifier, a thickener, a humectant, a penetration enhancer, and distilled water. The adhesive force is an important index for evaluating the quality of the hydrogel adhesive patch, and whether the patch can be firmly adhered to the surface of the skin is the key for effectively carrying out percutaneous absorption of the medicine. The adhesive force comprises initial adhesive force, permanent adhesive force and stripping force.
The earthworm syrup used as folk prescription for treating burns, scalds or sores and carbuncles has the problems of short shelf life, easy pathogenic microorganism generation or deterioration and the like when being used alone, thereby causing risks such as wound infection and the like, and can not play the role of anti-inflammation and sterilization on the burns, scalds or ulcerated wounds. And the earthworm syrup used alone needs repeated administration, is easy to pollute clothes, and is inconvenient for carrying and storing. The nano silver has the effects of sterilizing, diminishing inflammation and preventing infection on burn, scald or sore and carbuncle wounds, but cannot promote the healing of the wounds. And the nano silver can not be directly used for a ulceration wound, and if the nano silver is used for the ulceration wound or a mucous membrane, nano silver ions can easily pass through a human body barrier of the skin mucous membrane and circulate through blood, so that the nano silver can reach other organs and parts of a human body to be accumulated, and further liver cells and nerve cells can be damaged. When a large amount of silver ions are deposited in a human body, the silver ions can generate irreversible influence on the human body.
In the process of combining the earthworm syrup and the nano-silver, because the nano-silver is very fine powder and is difficult to be uniformly mixed in the earthworm syrup and the matrix, a new earthworm syrup product which ensures uniform distribution of the nano-silver in the earthworm syrup and the matrix is needed.
Disclosure of Invention
In view of the above, the invention provides a earthworm syrup nano-silver hydrogel patch and a preparation method thereof, aiming at the problems that the traditional earthworm syrup is not suitable for storage, is easy to deteriorate, is not easy to control quality, is inconvenient to use, is easy to pollute clothes, cannot play a role in resisting bacteria and diminishing inflammation, and cannot directly act on the wound surfaces of burns, scalds and sores and carbuncles due to nano-silver.
In order to solve the technical problem, the invention discloses a preparation method of a earthworm syrup nano-silver hydrogel patch, which comprises the following steps:
step 1, preparing earthworm syrup: soaking Lumbricus in clear water, cleaning soil, taking out, placing on absorbent paper, absorbing water to obtain pretreated Lumbricus, mixing pretreated Lumbricus with white sugar, standing, gradually precipitating body fluid to atrophy; centrifuging the mixture, filtering for 2-3 times, and collecting the extractive solution to obtain Lumbricus syrup;
step 2, preparing nano silver sol: putting nano silver into distilled water, and performing ultrasonic treatment to obtain nano silver sol;
step 3, preparing the earthworm syrup nano-silver hydrogel patch: the earthworm syrup nano-silver hydrogel patch is prepared by selecting sodium polyacrylate as a crosslinking framework, dihydroxyaluminum glycolate as a crosslinking agent, glycerin as a humectant, EDTA and tartaric acid as crosslinking regulators, carbomer, CMC-Na and PVPk30 as tackifiers and propylene glycol as penetration enhancers.
Optionally, the mass ratio of the pretreated earthworms to the white sugar is 1:0.6-1:1.6, and the standing time is 1.5-2.5 h.
Optionally, the mass-to-volume ratio (g/L) of the nano silver to the distilled water in the step 2 is 1:20-8:20, and the ultrasonic time is 5-15 min.
Optionally, the preparation of the earthworm syrup nano-silver hydrogel patch in the step 3 specifically comprises:
step 3.1, mixing glycerol and ethylene glycol, stirring, adding EDTA, fully stirring, adding dihydroxyaluminum glycolate, and fully stirring to obtain phase A;
step 3.2, uniformly mixing the sodium polyacrylate, the CMC-Na and the PVPK30 by an equivalent progressive mixing method to obtain a B phase;
step 3.3, adding carbomer into distilled water, and stirring the carbomer fully for later use as a phase C after the polymer is wetted;
step 3.4, sequentially dissolving tartaric acid and kaolin into distilled water, finally adding earthworm syrup and nano-silver sol, and fully stirring to obtain a phase D;
and 3.5, adding the phase B into the phase A under the stirring condition, adding the phase C into the phase AB mixed phase after 6min, stirring for 2min, finally adding the phase D, stirring for 20min, then uniformly coating the mixture on non-woven fabrics after ultrasonic degassing for 15min, drying for 0.5h, curing for 48h at room temperature, covering a back lining layer with the thickness of 1.5mm, sealing and packaging, and storing at room temperature.
Optionally, the mass ratio of the glycerol to the ethylene glycol in the step 3.1 is 4.5:1-5: 1; the mixing and stirring speed of the glycerol and the glycol is 230-280r/min, and the stirring time is 1-3 min; the mass ratio of EDTA to glycerol is 0.01:1-0.01: 1.5; the mass ratio of the dihydroxyaluminum glycinate to the glycerol is 1:48-2: 48; adding EDTA and aluminum glycollate, and stirring for 3-8 min.
Optionally, the mass ratio of the sodium polyacrylate, the CMC-Na and the PVPK30 in the step 3.2 is 12-15:3-8:1-5, and the mass ratio of the CMC-Na to the aluminum glycoxide is 1:0.1-1: 0.5.
Optionally, the mass ratio of carbomer to distilled water in step 3.3 is 0.2:15-0.6:15; the stirring speed is 280-320r/min, and the stirring time is 25-35min, wherein the mass ratio of the carbomer to the aluminum glyceroxide is 5:3-10: 3.
Optionally, the mass ratio of tartaric acid to kaolin in step 3.4 is 1:3 to 3: 3; the volume-to-mass ratio (ml/g) of the earthworm syrup to the tartaric acid is 1:0.02-1: 0.06; the volume-to-mass ratio (ml/g) of the nano silver sol to the tartaric acid is 1:0.1-1: 0.15; the stirring speed is 220-280r/min, the stirring time is 3-8min, and the mass ratio of the tartaric acid to the dihydroxyaluminum glycinate is 2:5-6: 5.
Optionally, the stirring speed in the step 3.5 is 220-280 r/min.
The invention also discloses the earthworm syrup nano-silver hydrogel patch prepared by the preparation method.
Compared with the prior art, the invention can obtain the following technical effects:
the earthworm syrup nano-silver hydrogel patch is prepared by adding antibacterial material nano-silver into earthworm syrup, and has strong combination, so that the earthworm syrup is efficient and safe and is not easy to generate drug resistance; the hydrogel patch is convenient and comfortable, does not pollute clothes, has high medicament utilization rate, has the moisture-keeping characteristic, plays a role in continuously cooling to help wound healing, improves the medicament effect and quality of products, provides a new idea for the development of traditional medicaments, and provides reference for the application of modern preparation technology on the traditional medicaments.
Of course, it is not necessary for any one product in which the invention is practiced to achieve all of the above-described technical effects simultaneously.
Detailed Description
The following embodiments are described in detail with reference to the accompanying drawings, so that how to implement the technical features of the present invention to solve the technical problems and achieve the technical effects can be fully understood and implemented.
The invention discloses a preparation method of a earthworm syrup nano-silver hydrogel patch, which comprises the following steps:
step 1, preparing earthworm syrup: soaking Lumbricus in clear water, cleaning soil, taking out, placing on absorbent paper, absorbing water to obtain pretreated Lumbricus, mixing pretreated Lumbricus with white sugar at a mass ratio of 1:0.6-1:1.6, standing for 1.5-2.5 hr to gradually precipitate body fluid and atrophy; centrifuging the mixture, filtering for 2-3 times, and collecting the extractive solution to obtain Lumbricus syrup;
step 2, preparing nano silver: placing nano silver in distilled water, and performing ultrasonic treatment for 5-15min to obtain nano silver sol; wherein the mass volume ratio (g/L) of the nano silver to the distilled water is 1:20-8: 20;
step 3, preparing the earthworm syrup nano-silver hydrogel patch: the earthworm syrup nano-silver hydrogel patch is prepared by selecting sodium polyacrylate as a crosslinking framework, dihydroxyaluminum glycolate as a crosslinking agent, glycerin as a humectant, EDTA and tartaric acid as crosslinking regulators, carbomer, CMC-Na and PVPk30 as tackifiers and propylene glycol as penetration enhancers.
Step 3.1, mixing glycerol and ethylene glycol and carrying out stirring treatment for 1-3min, wherein the stirring rotation speed is 230-280r/min, and the mass ratio of the glycerol to the ethylene glycol is 4.5:1-5: 1; sequentially adding EDTA and dihydroxyaluminum glycerolate, wherein the mass ratio of the EDTA to the glycerol is 0.01:1-0.01: 1.5; the mass ratio of the dihydroxyaluminum glycinate to the glycerol is 1:48-2: 48; stirring for 3-8min to obtain phase A;
step 3.2, uniformly mixing the sodium polyacrylate, the CMC-Na and the PVPK30 by an equivalent progressive mixing method to obtain a B phase; wherein the mass ratio of the sodium polyacrylate, the CMC-Na and the PVPK30 is 12-15:3-8:1-5, and the mass ratio of the CMC-Na to the aluminum glycoxide is 1:0.1-1: 0.5;
step 3.3, adding carbomer into distilled water, and using the carbomer as a C phase after the polymer is wetted and stirred for 25-35 min; wherein the mass ratio of carbomer to distilled water is 0.2:15-0.6:15; the mass ratio of carbomer to aluminum glyceroxide is 5:3-10: 3;
step 3.4, sequentially dissolving tartaric acid and kaolin into distilled water, finally adding earthworm syrup and nano-silver sol, and stirring at 280r/min for 3-8min for serving as a D phase; wherein the mass ratio of tartaric acid to kaolin is 1:3-3: 3; the volume-to-mass ratio (ml/g) of the earthworm syrup to the tartaric acid is 1:0.02-1: 0.06; the volume-to-mass ratio (ml/g) of the nano silver sol to the tartaric acid is 1:0.1-1: 0.15; the mass ratio of the tartaric acid to the dihydroxyaluminum glycinate is 2:5-6: 5;
and 3.5, adding the phase B into the phase A under the stirring condition of 280r/min for 220 plus, adding the phase C into the phase AB mixed phase after 6min, stirring for 2min, finally adding the phase D, stirring for 20min, then uniformly coating the mixture on non-woven fabrics after ultrasonic degassing for 15min, drying for 0.5h, curing for 48h at room temperature, covering a back lining with the thickness of 1.5mm, sealing and packaging, and storing at room temperature.
Example 1
(1) Preparing earthworm syrup: soaking Lumbricus in clear water to clean soil, taking out, placing on absorbent paper to absorb water, weighing 10g, adding into 50mL clean beaker, adding 5g white sugar, standing, and gradually precipitating body fluid to atrophy. Centrifuging the mixture after 2 hr, and filtering for 2-3 times to obtain filtrate, i.e. Lumbricus syrup.
(2) Preparing nano silver: placing nano silver in distilled water, and performing ultrasonic treatment for 10min to obtain nano silver sol; wherein the mass volume ratio (g/L) of the nano silver to the distilled water is 4: 20;
(3) preparation of hydrogel patch: sodium polyacrylate is used as a crosslinking framework, dihydroxyaluminum glycolate is used as a crosslinking agent, glycerin is used as a humectant, EDTA and tartaric acid are used as crosslinking regulators, carbomer, CMC-Na and PVPk30 are used as tackifiers, and propylene glycol is used as a penetration enhancer. Weighing 9.6g of glycerol and 2g of ethylene glycol in a clean beaker, stirring for 2min at 250r/min, sequentially adding 0.04g of EDTA and 0.15g of dihydroxyaluminum, and stirring for 5min respectively to obtain a phase A; weighing 1.34g of sodium polyacrylate, 0.5g of CMC-Na and 0.3g of PVPK30, and uniformly mixing by an equivalent progressive mixing method to obtain a phase B; weighing 0.4g of carbomer, adding into 15g of distilled water, and stirring for 30min at a speed of 300r/min after the polymer is wetted, wherein the carbomer is used as a phase C; weighing 0.12g of tartaric acid and 0.18g of kaolin, sequentially dissolving in distilled water, finally adding 3mL of earthworm syrup and 1mL of nano-silver sol, and stirring at 250r/min for 5min to obtain a D phase; adding phase B into phase A under stirring at 250r/min, adding phase C into phase AB mixed phase, stirring for 2min, adding phase D, stirring for 20min, ultrasonic degassing for 15min, uniformly coating on non-woven fabric, oven drying for 0.5 hr, curing at room temperature for 48 hr, covering with backing cloth to a thickness of 1.5mm, sealing, packaging, and storing at room temperature.
Example 2
Step 1, preparing earthworm syrup: soaking Lumbricus in clear water, cleaning soil, taking out, placing on absorbent paper, absorbing water to obtain pretreated Lumbricus, mixing pretreated Lumbricus with white sugar at a mass ratio of 1:0.6, standing for 2.5 hr to gradually separate body fluid and atrophy; centrifuging the mixture, filtering for 2-3 times, and collecting the extractive solution to obtain Lumbricus syrup;
step 2, preparing nano silver: placing nano silver in distilled water, and performing ultrasonic treatment for 15min to obtain nano silver sol; wherein the mass volume ratio (g/L) of the nano silver to the distilled water is 1: 20;
step 3, preparing the earthworm syrup nano-silver hydrogel patch: the earthworm syrup nano-silver hydrogel patch is prepared by selecting sodium polyacrylate as a crosslinking framework, dihydroxyaluminum glycolate as a crosslinking agent, glycerin as a humectant, EDTA and tartaric acid as crosslinking regulators, carbomer, CMC-Na and PVPk30 as tackifiers and propylene glycol as penetration enhancers.
Step 3.1, mixing glycerol and ethylene glycol, stirring for 1min at the stirring speed of 280r/min, wherein the mass ratio of the glycerol to the ethylene glycol is 4.5: 1; sequentially adding EDTA and dihydroxyaluminum glycerolate, wherein the mass ratio of the EDTA to the glycerol is 0.01: 1.5; the mass ratio of the dihydroxyaluminum glycinate to the glycerol is 1: 48; stirring for 8min respectively to obtain phase A;
step 3.2, uniformly mixing the sodium polyacrylate, the CMC-Na and the PVPK30 by an equivalent progressive mixing method to obtain a B phase; wherein the mass ratio of the sodium polyacrylate, the CMC-Na and the PVPK30 is 12:8:1, and the mass ratio of the CMC-Na to the dihydroxyaluminum glycinate is 1: 0.5;
step 3.3, adding carbomer into distilled water, and after the polymer is wetted and stirred for 25min, using the carbomer as a phase C; wherein the mass ratio of carbomer to distilled water is 0.6:15; the mass ratio of carbomer to aluminum glyceroxide is 5: 3;
step 3.4, sequentially dissolving tartaric acid and kaolin into distilled water, finally adding earthworm syrup and nano-silver sol, and stirring at 280r/min for 3min to obtain a D phase; wherein the mass ratio of tartaric acid to kaolin is 1: 3; the volume-to-mass ratio (ml/g) of the earthworm syrup to the tartaric acid is 1: 0.06; the volume-to-mass ratio (ml/g) of the nano silver sol to the tartaric acid is 1: 0.1; the mass ratio of the tartaric acid to the dihydroxyaluminum glycinate is 6: 5;
and 3.5, adding the phase B into the phase A under the stirring condition of 220r/min, adding the phase C into the phase AB mixed phase after 6min, stirring for 2min, finally adding the phase D, stirring for 20min, then uniformly coating the mixture on non-woven fabrics after ultrasonic degassing for 15min, drying for 0.5h, curing for 48h at room temperature, covering a back lining with the thickness of 1.5mm, sealing and packaging, and storing at room temperature.
Example 3
Step 1, preparing earthworm syrup: soaking Lumbricus in clear water, cleaning soil, taking out, placing on absorbent paper, absorbing water to obtain pretreated Lumbricus, mixing pretreated Lumbricus with white sugar at a mass ratio of 1:1.6, standing for 1.5 hr to gradually separate body fluid and atrophy; centrifuging the mixture, filtering for 2-3 times, and collecting the extractive solution to obtain Lumbricus syrup;
step 2, preparing nano silver: placing nano silver in distilled water, and performing ultrasonic treatment for 5min to obtain nano silver sol; wherein the mass volume ratio (g/L) of the nano silver to the distilled water is 8: 20;
step 3, preparing the earthworm syrup nano-silver hydrogel patch: the earthworm syrup nano-silver hydrogel patch is prepared by selecting sodium polyacrylate as a crosslinking framework, dihydroxyaluminum glycolate as a crosslinking agent, glycerin as a humectant, EDTA and tartaric acid as crosslinking regulators, carbomer, CMC-Na and PVPk30 as tackifiers and propylene glycol as penetration enhancers.
Step 3.1, mixing glycerol and ethylene glycol and carrying out stirring treatment for 3min, wherein the stirring speed is 230r/min, and the mass ratio of the glycerol to the ethylene glycol is 5: 1; sequentially adding EDTA and dihydroxyaluminum glycerolate, wherein the mass ratio of the EDTA to the glycerol is 0.01: 1; the mass ratio of the dihydroxyaluminum glycinate to the glycerol is 2: 48; stirring for 3min respectively to obtain phase A;
step 3.2, uniformly mixing the sodium polyacrylate, the CMC-Na and the PVPK30 by an equivalent progressive mixing method to obtain a B phase; wherein the mass ratio of the sodium polyacrylate, the CMC-Na and the PVPK30 is 15:3:5, and the mass ratio of the CMC-Na to the dihydroxyaluminum glycinate is 1: 0.1;
step 3.3, adding carbomer into distilled water, and stirring the dispersion liquid for 35min after the polymer is wetted for later use as a C phase; wherein the mass ratio of carbomer to distilled water is 0.2: 15; the mass ratio of carbomer to aluminum glyceroxide is 10: 3;
step 3.4, sequentially dissolving tartaric acid and kaolin into distilled water, finally adding earthworm syrup and nano-silver sol, and stirring for 8min at 220r/min to obtain a D phase; wherein the mass ratio of tartaric acid to kaolin is 1:3-3: 3; the volume-to-mass ratio (ml/g) of the earthworm syrup to the tartaric acid is 1: 0.02; the volume-to-mass ratio (ml/g) of the nano silver sol to the tartaric acid is 1: 0.15; the mass ratio of the tartaric acid to the dihydroxyaluminum glycinate is 2: 5;
and 3.5, adding the phase B into the phase A under the stirring condition of 280r/min, adding the phase C into the phase AB mixed phase after 6min, stirring for 2min, finally adding the phase D, stirring for 20min, then uniformly coating the mixture on non-woven fabrics after ultrasonic degassing for 15min, drying for 0.5h, curing for 48h at room temperature, covering a back lining with the thickness of 1.5mm, sealing and packaging, and storing at room temperature.
Comparative example 1
Commercially available Lumbricus syrup is used.
The technical effects of the present invention are explained below with reference to specific experimental data:
1. initial adhesion measurement and evaluation: the sample is placed in the center of a 30-degree inclined plate, the plaster surface of the sample is upward, 10cm at the upper part and 15cm at the lower part of the inclined plate are covered by thick polyester films, 5cm plaster surface is reserved in the middle, steel balls under various specifications are freely rolled down from the 30-degree inclined plate, the largest steel ball which can be stuck by the plaster surface of the cataplasm is observed, and the initial adhesion force of the steel balls is evaluated. And (4) preselecting larger steel balls, observing whether the rolled steel balls can be stuck in the test section (stopping moving for more than 5 seconds), and performing tests by using steel balls of different types from large to small until the steel ball with the largest size stuck in the test section is found. The steel ball having the largest ball number capable of being stuck and two balls having sizes adjacent to the steel ball are taken and subjected to a test on the same sample to confirm the largest ball number of the steel ball. The scoring criteria are shown in table 1.
TABLE 1 initial adhesion force scoring standard table
Figure BDA0001859258760000101
The initial tack measurements and evaluations of examples 1-3 and comparative example 1 are shown in Table 2.
TABLE 2 initial tack measurement and evaluation of examples 1 to 3 and comparative example 1
Initial adhesion rating (score)
Example 1 85
Example 2 88
Example 3 84
Comparative example 1 73
2. And (4) measuring and evaluating the permanent adhesive force. Before the test, the sample backing was removed so as not to overlap with each other and left at room temperature for 2 hours or more. Cleaning the experimental plate and the loading plate by using a wiping material, then wiping the experimental plate and the loading plate by using clean gauze, and repeatedly cleaning for more than three times until the working surface of the plate is cleaned, wherein the cleaned plate surface cannot be contacted by hands or other objects. The test sample is longitudinally pasted in the middle of the experiment plate and the loading plate which are next to each other, the press roller rolls the test sample back and forth three times, the test sample is placed for 20 minutes after being pasted on the plate, the test sample is fixed on the experiment frame after being added with 200g of weight, and the initial time of the test is recorded. The scoring criteria are shown in table 3.
TABLE 3 standard table for evaluation of permanent adhesion
Figure BDA0001859258760000102
Figure BDA0001859258760000111
The tack scores for examples 1-3 and comparative example 1 are shown in Table 4.
TABLE 4 Holset adhesion scores for examples 1-3 and comparative example 1
Hand-held adhesive force score (score)
Example 1 83
Example 2 86
Example 3 85
Comparative example 1 55
3. And (4) measuring and evaluating the peeling force. Removing the anti-sticking layer on the surface of the hydrogel patch (10cm multiplied by 10cm), sticking the hydrogel patch on a clean steel plate, and rolling the hydrogel patch back and forth for several times by using a 2kg round ball; uncovering one end (about 2cm) of the hydrogel patch after 10min, and clamping with a spring balance (180 DEG from a steel plate); the hydrogel patch was then peeled off at a rate, and the peel force was recorded 1 time at 5s intervals, and the average of 3 consecutive peel forces was used as a measure. The scoring criteria are shown in table 5.
TABLE 5 Peel force score criteria Table
Figure BDA0001859258760000112
The peel force scores for examples 1-3 and comparative example 1 are shown in Table 6.
TABLE 6 Peel force scores for examples 1-3 and comparative example 1
Figure BDA0001859258760000113
Figure BDA0001859258760000121
4. Appearance evaluation: the paste is stirred for difficulty and viscosity; observing whether the surface of the prepared patch is smooth, bubble-free or particle-free; the appearance of the hydrogel patch was evaluated by observing whether the backing layer was exuded or not and whether the patch remained on the skin, and the evaluation criteria are shown in Table 7.
Table 7 appearance scoring criteria table
Figure BDA0001859258760000122
The appearance of the earthworm syrup nanosilver hydrogel patches prepared in examples 1-3 and comparative example 1 was evaluated as shown in Table 8.
TABLE 8 evaluation of appearance of Lumbricus syrup nanosilver hydrogel patch prepared in examples 1-3 and comparative example 1
Figure BDA0001859258760000123
Figure BDA0001859258760000131
While the foregoing description shows and describes several preferred embodiments of the invention, it is to be understood, as noted above, that the invention is not limited to the forms disclosed herein, but is not to be construed as excluding other embodiments and is capable of use in various other combinations, modifications, and environments and is capable of changes within the scope of the inventive concept as expressed herein, commensurate with the above teachings, or the skill or knowledge of the relevant art. And that modifications and variations may be effected by those skilled in the art without departing from the spirit and scope of the invention as defined by the appended claims.

Claims (4)

1. A preparation method of a earthworm syrup nano-silver hydrogel patch is characterized by comprising the following steps:
step 1, preparing earthworm syrup: soaking Lumbricus in clear water, cleaning soil, taking out, placing on absorbent paper, absorbing water to obtain pretreated Lumbricus, mixing pretreated Lumbricus with white sugar, standing, gradually precipitating body fluid to atrophy; centrifuging the mixture, filtering for 2-3 times, and collecting the extractive solution to obtain Lumbricus syrup;
step 2, preparing nano silver sol: putting nano silver into distilled water, and performing ultrasonic treatment to obtain nano silver sol;
step 3, preparing the earthworm syrup nano-silver hydrogel patch: selecting sodium polyacrylate as crosslinking skeleton, dihydroxyaluminum glycolate as crosslinking agent, glycerol as humectant, EDTA and tartaric acid as crosslinking regulator, carbomer, CMC-Na and PVPk30 as tackifier, and propylene glycol as penetration promoter, and making into Lumbricus syrup nanometer silver hydrogel patch;
the preparation of the earthworm syrup nano-silver hydrogel patch in the step 3 specifically comprises the following steps:
step 3.1, mixing glycerol and ethylene glycol, stirring, adding EDTA, fully stirring, adding dihydroxyaluminum glycolate, and fully stirring to obtain phase A;
step 3.2, uniformly mixing the sodium polyacrylate, the CMC-Na and the PVPK30 by an equivalent progressive mixing method to obtain a B phase;
step 3.3, adding carbomer into distilled water, and stirring the carbomer fully for later use as a phase C after the polymer is wetted;
step 3.4, sequentially dissolving tartaric acid and kaolin into distilled water, finally adding earthworm syrup and nano-silver sol, and fully stirring to obtain a phase D;
step 3.5, adding the phase B into the phase A under the stirring condition, adding the phase C into the phase AB mixed phase after 6min, stirring for 2min, finally adding the phase D, stirring for 20min, then ultrasonically degassing for 15min, uniformly coating the mixture on non-woven fabric, drying for 0.5h, curing at room temperature for 48h, covering a back lining layer with the thickness of 1.5mm, sealing and packaging, and storing at room temperature;
the mass ratio of the glycerol to the ethylene glycol in the step 3.1 is 4.5:1-5: 1; the mixing and stirring speed of the glycerol and the glycol is 230-280r/min, and the stirring time is 1-3 min; the mass ratio of EDTA to glycerol is 0.01:1-0.01: 1.5; the mass ratio of the dihydroxyaluminum glycinate to the glycerol is 1:48-2: 48; adding EDTA and aluminum glycollate, and stirring for 3-8 min;
the mass ratio of the pretreated earthworms to the white sugar is 1:0.6-1:1.6, and the standing time is 1.5-2.5 h;
the mass ratio of the sodium polyacrylate, the CMC-Na and the PVPK30 in the step 3.2 is 12-15:3-8:1-5, and the mass ratio of the CMC-Na to the aluminum glycoxide is 1:0.1-1: 0.5;
the mass ratio of the carbomer to the distilled water in the step 3.3 is 0.2:15-0.6:15, the stirring rotation speed is 280-320r/min, and the stirring time is 25-35min, wherein the mass ratio of the carbomer to the aluminum glycoxide is 5:3-10: 3;
the mass ratio of the tartaric acid to the kaolin in the step 3.4 is 1:3-3: 3; the volume-to-mass ratio (ml/g) of the earthworm syrup to the tartaric acid is 1:0.02-1: 0.06; the volume-to-mass ratio (ml/g) of the nano silver sol to the tartaric acid is 1:0.1-1: 0.15; the stirring speed is 220-280r/min, the stirring time is 3-8min, and the mass ratio of the tartaric acid to the dihydroxyaluminum glycinate is 2:5-6: 5.
2. The preparation method according to claim 1, wherein the mass-to-volume ratio (g/L) of the nano silver to the distilled water in the step 2 is 1:20-8:20, and the ultrasonic time is 5-15 min.
3. The method as claimed in claim 1, wherein the stirring speed in step 3.5 is 220-280 r/min.
4. A Lumbricus syrup nanosilver hydrogel patch prepared by the preparation method of any one of claims 1-3.
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