CN114904041A

CN114904041A - Medical dressing based on humifuse euphorbia herb extract and preparation method thereof

Info

Publication number: CN114904041A
Application number: CN202210608708.XA
Authority: CN
Inventors: 李剑峰; 丁梦雅; 满佳; 李建勇; 华泽升; 彭思贤; 张永琪
Original assignee: Shandong University
Current assignee: Shandong University
Priority date: 2022-05-31
Filing date: 2022-05-31
Publication date: 2022-08-16
Anticipated expiration: 2042-05-31
Also published as: CN114904041B

Abstract

The invention relates to a medical dressing based on humifuse euphorbia herb extract and a preparation method thereof. The degradable composite fiber dressing is prepared by utilizing alginate and humifuse euphorbia herb extract components. The invention extracts flavonoid compound material from humifuse euphorbia herb, and mixes the flavonoid compound material with sodium alginate, PVA and microcrystalline cellulose according to a certain proportion, and then the degradable composite fiber dressing with good mechanical property and physical property is prepared by calcium ion crosslinking treatment. By utilizing the method, the green, nontoxic and biodegradable medical dressing material with good mechanical property and physical property can be efficiently prepared, and the problem of environmental pollution caused by burning medical wastes can be relieved to a certain extent.

Description

Medical dressing based on humifuse euphorbia herb extract and preparation method thereof

Technical Field

The invention belongs to the technical field of medical dressings, and particularly relates to a medical dressing based on a humifuse euphorbia herb extract and a preparation method thereof.

Background

The information in this background section is only for enhancement of understanding of the general background of the invention and is not necessarily to be construed as an admission or any form of suggestion that this information forms the prior art that is already known to a person of ordinary skill in the art.

The alginate fiber dressing has the excellent performances of large aperture ratio, good hygroscopicity, easy removal and the like. The alginate fiber dressing is mainly used for nursing burn wounds and moderately severe weeping wounds in clinic. However, the antibacterial property, hemostatic property, mechanical property and the like of alginate fiber dressing still need to be further improved.

The humifuse euphorbia herb is a plant of euphorbiaceae and is a Chinese herbal medicine with remarkable curative effect. It is recorded in Song 'Ben Cao gang mu'. The humifuse euphorbia herb has vigorous vitality, wide source and rich resources. The humifuse euphorbia herb mainly contains quercitrin glycosides, kaempferol glycosides and other flavonoid compounds, has the effects of cooling blood and stopping bleeding, clearing heat and detoxicating, promoting diuresis and removing jaundice and the like, and pharmacological research proves that the flavonoid compounds are the main effective components of the humifuse euphorbia herb for resisting bacteria, stopping bleeding and resisting oxidation. Currently, there are few reports of polysaccharide-based fibrous dressings with antibacterial hemostatic properties for infected wound repair.

Disclosure of Invention

Aiming at the problems in the prior art, the invention provides a medical dressing based on a humifuse euphorbia herb extract and a preparation method thereof. The degradable composite fiber dressing is prepared by utilizing alginate and humifuse euphorbia herb extract components. The invention extracts flavonoid compound material from humifuse euphorbia herb, and mixes the flavonoid compound material with sodium alginate, PVA and microcrystalline cellulose according to a certain proportion, and then prepares the degradable composite fiber dressing with good mechanical property and physical property through calcium ion crosslinking treatment. The degradable composite fiber dressing has good mechanical property, air permeability, antibacterial property and blood coagulation property.

In order to achieve the purpose, the invention adopts the following technical scheme:

a preparation method of a medical dressing based on humifuse euphorbia herb extract comprises the following steps:

(1) extracting humifuse euphorbia herb: cutting dry humifuse euphorbia herb into short fiber sections, soaking and cleaning, drying, pouring into a grinder to be ground into particles, soaking and then carrying out reflux extraction; filtering, extracting the filter residue under reflux again, and mixing the two herba Euphorbiae Humifusae extractive solutions;

(2) preparation of spinning solution: diluting the obtained humifuse euphorbia herb extract to a proper concentration, adding a mixture of sodium alginate, PVA and microcrystalline cellulose, heating in a water bath, and uniformly stirring to obtain an inner phase solution; adding deionized water into anhydrous calcium chloride particles, and uniformly shaking to obtain an external phase solution;

(3) preparation of the composite fiber dressing: carrying out suction filtration on the internal phase solution and the external phase solution to remove bubbles; taking the inner phase solution as a core solution and the outer phase solution as a sheath solution; the core liquid and the sheath liquid are extruded into a channel of the microfluidic chip through an injection pump, and the sodium alginate and the calcium ions are crosslinked to form calcium alginate hydrogel microfibers; and assembling the calcium alginate hydrogel microfibers into a grid structure by adopting a plain weaving process, and folding to obtain the composite fiber dressing.

The grid structure is obtained through the plain weaving process, the area of the grid structure is large, the holes are large and loose, the thickness of the dressing can be increased through folding, the area is reduced, and the pores of the dressing after folding are more compact.

Further, the length of the short fiber section is 1-2 cm.

Further, soaking and reflux extraction are carried out by adopting distilled water; the soaking time is 12 h; the time for two reflux extractions is 1 h.

Further, the water bath heating temperature is 80-85 ℃, and the time is 2 h.

Further, the concentration in the step (2) is 0.2 wt% to 1 wt%. The using amount ratio of the humifuse euphorbia herb extract to the mixture of sodium alginate, PVA and microcrystalline cellulose is 50mL:2g:2.5g:0.2 g.

Further, the mass ratio of the anhydrous calcium chloride particles to the deionized water in the step (2) is 1: 49.

furthermore, the microfluidic chip is composed of two cylindrical glass capillaries which are coaxially arranged and are respectively called an injection tube and a collecting tube; the preparation method of the microfluidic chip comprises the following steps: tapering a circular capillary tube with the inner diameter of 300 mu m to a required hole opening by using a micro-tube puller and a micro-forging furnace to form a conical capillary tube, namely the injection tube; a tapered capillary (syringe) is inserted into the collection tube, the syringe serving as the core flow channel and the collection tube as the sheath flow channel need to be coated with a hydrophobic reagent (OTS). Where necessary, a clear epoxy is used to seal the tubing.

Further, the inner diameter of the collecting pipe is 1.0mm, and the length of the collecting pipe is 65 mm; the maximum inner diameter of the injection tube is 300 mu m, the minimum inner diameter at the conical outlet is 80 mu m, and the length is 55 mm.

Further, respectively filling the internal and external phase solution into two 10ml syringes, fixing the two syringes on an injection pump, and setting the solution amount and flow rate; connecting the microfluidic chip with a polyethylene tube; the microfluidic chip is fixed to be vertically placed, a collection culture dish is placed at the rear end of the microfluidic chip, and a calcium chloride solution is placed in the culture dish to serve as a collection liquid.

The medical dressing based on the humifuse euphorbia herb extract is prepared by the method.

Compared with the prior art, the invention has the following beneficial effects:

the invention provides a preparation method of a fiber dressing, which takes sodium alginate as a composite matrix, microcrystalline cellulose and PVA as reinforcement, humifuse euphorbia herb as a functional material and calcium chloride as a cross-linking agent, and the performance of the prepared dressing is superior to that of gauze traditional medical dressings.

By utilizing the method, the green, nontoxic and biodegradable medical dressing material with good mechanical property and physical property can be efficiently prepared, and the problem of environmental pollution caused by burning medical wastes can be relieved to a certain extent.

The method provided by the invention is based on a macromolecule bonding theory, and can be used for simply and controllably preparing composite fiber type dressings with different performances. By changing the content of sodium alginate, the content of microcrystalline cellulose and the content of PVA, the composite dressing material with different water absorption rates, water vapor transmission rates and mechanical properties can be prepared more accurately. By changing the content of the humifuse euphorbia herb extract, the composite dressing material with different antibacterial rates and blood coagulation effects can be accurately prepared.

The method provided by the invention is scientific, reasonable, simple and feasible, does not cause harm to the environment by the production process, and combines the concepts of green manufacturing and sustainable development.

Drawings

The accompanying drawings, which are incorporated in and constitute a part of this specification, are included to provide a further understanding of the invention, and are incorporated in and constitute a part of this specification, illustrate exemplary embodiments of the invention and together with the description serve to explain the invention and not to limit the invention.

Fig. 1 is a schematic flow chart of the preparation of the biomass composite fiber dressing according to the invention.

Fig. 2 is a schematic diagram of a structure of a microfluidic device prepared according to the present invention and a diagram of a microfluidic chip and a microfluidic device.

FIG. 3 is a pictorial representation of examples 1-5 prepared in accordance with the present invention.

Fig. 4 is a graph comparing the antibacterial performance of the composite dressings prepared in examples 1-5 of the present invention with that of a blank control group.

FIG. 5 is a graph comparing the clotting properties of the composite dressings prepared in examples 1-5 of the present invention and a film of the same material.

FIG. 6 is a graph comparing the swelling and breathability performance of composite dressings prepared in examples 1-5 of the present invention with films of the same materials and gauze.

Detailed Description

It is to be understood that the following detailed description is exemplary and is intended to provide further explanation of the invention as claimed. Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs.

The invention will now be further described with reference to the accompanying drawings and detailed description.

Example 1

A preparation method of a medical dressing based on herba Euphorbiae Humifusae extract comprises the following steps (see figure 1 for preparation process):

(1) extracting humifuse euphorbia herb: cutting 10g of dried humifuse euphorbia herb into 1-2cm short fiber sections, weighing 10g of short fiber sections, soaking the short fiber sections in absolute ethyl alcohol solution for cleaning, filtering and placing for 24h for drying, pouring the cleaned and dried humifuse euphorbia herb fibers into a grinder, beating the fibers into micron-sized particles, collecting the particles in a beaker, adding 200ml of distilled water for soaking for 12h, and carrying out reflux extraction on the humifuse euphorbia herb solution at 95 ℃ for 1 h. Filtering with 400 mesh filter screen, placing the filter residue into beaker again, adding 200ml distilled water, reflux extracting for 1h, mixing the two extractive solutions, and measuring the mass concentration of the solution.

(2) Preparation of spinning solution: diluting the humifuse euphorbia extract solution obtained in the step (1) to the concentration of 0.2 wt% of the matrix content, taking 50mL of the humifuse euphorbia extract solution, then adding a mixture of 2g of sodium alginate, 2.5g of PVA and 0.2g of microcrystalline cellulose into the solution, heating and stirring the mixture in a water bath kettle at the temperature of 80 ℃ for 2 hours, and uniformly mixing the solution to obtain an inner phase solution; 1g of anhydrous calcium chloride particles are placed in a centrifuge tube, 49g of deionized water is added, and the centrifuge tube is uniformly shaken to obtain an external phase solution.

(3) Preparation of microfluidic chip (microfluidic chip see fig. 2): the capillary microfluidic device is composed of two cylindrical glass capillaries which are coaxially arranged and are respectively called an injection tube and a collecting tube. A circular capillary tube with an inner diameter of 300um was tapered to an orifice with a diameter of about 80um using a microtube puller and a microcalciner. The tapered capillary tube was cut with a glass cutter to a length of 55mm to form an injection tube, and a capillary glass tube having an inner diameter of 1.0mm was cut with a glass cutter to a length of 65mm to form a collection tube. A glass tube is placed on a 20mm by 50mm transparent glass slide, and a tapered capillary (syringe) is inserted into the collection tube, the syringe serving as the core flow channel and the collection tube serving as the sheath flow channel need to be coated with a hydrophobic reagent (OTS). Where necessary, a clear epoxy is used to seal the duct.

(4) Preparation of the microfluidic spinning device (microfluidic spinning device see fig. 2): and (4) carrying out suction filtration on the solution prepared in the step, and removing air bubbles in the solution. The internal and external phase solution is respectively filled into two 10ml syringes, the two syringes are fixed on an injection pump, and the flow rates are respectively set to be 2ml/h and 20 ml/h. Polyethylene tubing was used to connect to the microfluidic chip. The chip was fixed in a vertical position, a collection petri dish with a diameter of 8cm was placed under the chip, and 2 wt% calcium chloride solution was placed in the petri dish as a collection solution.

(5) Preparation of the composite fiber dressing: a mixed solution of PVA, microcrystalline cellulose, humifuse euphorbia herb and alginate is selected as a core solution, and anhydrous calcium chloride is added into deionized water to reach the concentration of 2 wt% to be used as a sheath solution. The core flow and the sheath flow are extruded into a channel of the microfluidic chip through a syringe pump, and the sodium alginate solution and calcium ions are crosslinked to form the calcium alginate hydrogel microfiber. Cutting the fibers according to 10cm, wherein 100 fibers are used as warps and 100 fibers are used as wefts, assembling the fibers into a grid structure by adopting a plain weaving process, and folding to obtain a final finished product.

Example 2

This example is substantially the same as example 1 except that:

in this embodiment, the step (2) specifically includes: diluting the humifuse euphorbia extract solution obtained in the step (1) to the concentration of 0.2 wt%, taking 50ml of humifuse euphorbia extract solution, then adding a mixture of 2g of sodium alginate, 2.5g of PVA and 0.2g of microcrystalline cellulose into the solution, heating and stirring the mixture in a water bath kettle at the temperature of 85 ℃ for 2 hours, and uniformly mixing the solution to obtain an inner phase solution; putting 1g of anhydrous calcium chloride particles into a centrifuge tube, adding 49g of deionized water, and uniformly shaking to obtain an external phase solution.

Example 3

This example is substantially the same as example 1, except that:

in this embodiment, the step (2) specifically includes: diluting the humifuse euphorbia extract solution obtained in the step (1) to the concentration of 0.5 wt%, taking 50ml of humifuse euphorbia extract solution, then adding a mixture of 2g of sodium alginate, 2.5g of PVA and 0.2g of microcrystalline cellulose into the solution, heating and stirring the mixture in a water bath kettle at the temperature of 80 ℃ for 2 hours, and uniformly mixing the solution to obtain an inner phase solution; 1g of anhydrous calcium chloride particles are placed in a centrifuge tube, 49g of deionized water is added, and the centrifuge tube is uniformly shaken to obtain an external phase solution.

Example 4

This example is substantially the same as example 1 except that:

in this embodiment, the step (2) specifically includes: diluting the humifuse euphorbia extract solution obtained in the step (1) to the concentration of 0.8 wt%, taking 50ml of humifuse euphorbia extract solution, then adding a mixture of 2g of sodium alginate, 2.5g of PVA and 0.2g of microcrystalline cellulose into the solution, heating and stirring the mixture in a water bath kettle at the temperature of 85 ℃ for 2 hours, and uniformly mixing the solution to obtain an inner phase solution; 1g of anhydrous calcium chloride particles are placed in a centrifuge tube, 49g of deionized water is added, and the centrifuge tube is uniformly shaken to obtain an external phase solution.

Example 5

This example is substantially the same as example 1 except that:

in this embodiment, the step (2) specifically includes: diluting the humifuse euphorbia extract solution obtained in the step (1) to the concentration of 1 wt%, taking 50ml of the humifuse euphorbia extract solution, then adding a mixture of 2g of sodium alginate, 2.5g of PVA and 0.2g of microcrystalline cellulose into the solution, heating and stirring the mixture in a water bath kettle at the temperature of 85 ℃ for 2 hours, and uniformly mixing the solution to obtain an inner phase solution; 1g of anhydrous calcium chloride particles are placed in a centrifuge tube, 49g of deionized water is added, and the centrifuge tube is uniformly shaken to obtain an external phase solution.

Comparative example: film prepared by same solution by using tape casting film forming process and calcium ion crosslinking and commercial medical gauze

The composite fiber type dressings obtained in examples 1 to 5 were tested by the following specific test methods: and (3) determining the antibacterial activity of the humifuse euphorbia herb extracts with different concentrations on the samples by adopting a colony counting method. Escherichia coli and Staphylococcus aureus are used as role models of gram-negative bacteria and gram-positive bacteria, respectively. The bacteria were inoculated into a test tube and shaken at 37 ℃ for 24 hours to prepare a culture of about 105CFU/ml of the strain for evaluation of antibacterial activity. Dressing samples were cut into 5mm diameter circles and sterilized with uv radiation for 30 minutes. Then, 1ml of the inoculum (105CFU/ml) was added to the sample, and the sample was incubated at 37 ℃ for 24 hours. After incubation, 10ml of sterile deionized water was added and the bacteria were eluted from the sample by vigorous shaking at room temperature for 5 min. The eluate was then serially diluted with 0.1% w/v peptone. 100ul of each diluted solution was spread on nutrient agar plates and incubated at 37 ℃ for 24 h. Finally, counting colonies, and calculating the inhibition rate (R,%) according to the number of colonies of a control group without a sample.

Where A is the number of bacteria recovered after 24 hours incubation at 37 ℃ for the sample and B is the number of bacteria recovered after 24 hours incubation at 37 ℃ for the control (no sample).

The composite fiber type dressings and comparative examples obtained in examples 1 to 5 were tested by the following specific test methods: the calcium alginate fiber dressing and the medical gauze are cut into a square shape of 1cm multiplied by 1cm and are placed into a beaker. The mixture was then washed with water at 37 ℃ for 5 min. 5ml of fresh sodium citrate anticoagulated blood is mixed with 150ul of 0.1M/L calcium chloride solution, 100ul of mixed blood is slowly added to each group of samples, and after incubation for 5min, 20ml of deionized water is slowly added. The absorbance (A) of the supernatant was measured at 545nm by spectrophotometry. The in vitro coagulation index (BCI) values of each group of materials were calculated according to the following formula: (absorbance of 100ul of mixed blood mixed with 20ml of deionized water was used as a reference value)

The composite fiber dressing obtained in example 5 and the comparative example were tested by the following specific test methods: the water swelling and weight loss behavior of dressings, films and gauzes were determined gravimetrically. Dressing, film and gauze samples were cut to 2.0cm by 2.0cm in size, soaked in Phosphate Buffered Saline (PBS) at 37 ℃ for 30min at pH 7.2-7.4, then the residual PBS was removed from the wet sample surface with filter paper and the resulting samples were immediately weighed. The measured value for each sample was calculated as follows:

where M is the weight of each sample after soaking in the buffer solution, and Md is the weight of each sample in a dry state.

The composite fiber dressing obtained in example 1 and the comparative example were tested by the following specific test methods: the air permeability of the composite film was measured by cup method at 37. + -. 0.5 ℃ and relative humidity of 90. + -. 2% for the sample. A25 mm by 25mm test membrane specimen was fixed with an all-purpose adhesive to the opening of a glass bottle containing 5ml of deionized water. The evaporation of water through the test membrane was monitored by measuring the water loss from the system at 37 ℃. The water vapor transmission rate of the sample was determined by the following formula

WVT means air permeability per square meter per hour, g/m 2. h; Δ m is the mass difference of the cup before and after the test, g; s is the effective area of the membrane, i.e. the area of the glass bottle opening, m 2; t is the test time, days. Each test was repeated 3 times and the average was taken.

Fig. 3 is a physical diagram of examples 1-5 prepared by the present invention, and it can be seen that the color of the surface of the dressing gradually deepens with the increase of the humifuse euphorbia herb extract.

Fig. 4 is a comparison graph of the antibacterial performance of the composite dressing prepared in examples 1-5 of the present invention and a blank control group, and it can be seen from fig. 4 that the dressing prepared by the present invention has good antibacterial performance. Wherein, the bacteriostatic activity of the example 5 is more than 99.99 percent.

FIG. 5 is a graph comparing the blood coagulation performance of the composite dressings prepared in examples 1 to 5 of the present invention with that of a film of the same material, and the lower the BCI value, the better the blood coagulation performance. It can be seen that the film prepared by the invention has good blood coagulation and hemostasis performance.

Fig. 6 is a graph comparing the swelling and breathability properties of the composite dressing prepared in example 1 of the present invention with a film of the same material and gauze. It can be seen that the dressing prepared by the invention has good moisture absorption swelling capacity and air permeability.

It should be noted that the above-mentioned embodiments are only preferred embodiments of the present invention, and the present invention is not limited thereto, and although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that modifications and equivalents can be made in the technical solutions described in the foregoing embodiments, or equivalents thereof. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention. Although the present invention has been described with reference to the specific embodiments, it should be understood by those skilled in the art that various changes and modifications may be made without departing from the spirit and scope of the invention.

Claims

1. A preparation method of a medical dressing based on humifuse euphorbia herb extract is characterized by comprising the following steps:

2. The method according to claim 1, wherein the soaking and reflux extraction are carried out with distilled water; the soaking time is 12 h; the time for two reflux extractions is 1 h.

3. The method according to claim 1, wherein the concentration in the step (2) is 0.2 wt% to 1 wt%; the using amount ratio of the humifuse euphorbia herb extract to the mixture of sodium alginate, PVA and microcrystalline cellulose is 50mL:2g:2.5g:0.2 g.

4. The preparation method according to claim 1, wherein the mass ratio of the anhydrous calcium chloride particles to the deionized water in the step (2) is 1: 49.

5. the preparation method according to claim 1, wherein the microfluidic chip is composed of two cylindrical glass capillaries which are coaxially arranged and are respectively called an injection tube and a collection tube; the preparation method of the microfluidic chip comprises the following steps: tapering a circular capillary tube with the inner diameter of 300 mu m to a required hole opening by using a micro-tube puller and a micro-forging furnace to form a conical capillary tube, namely the injection tube; a tapered capillary (syringe) is inserted into the collection tube, the syringe serving as the core flow channel and the collection tube as the sheath flow channel need to be coated with a hydrophobic reagent.

6. The preparation method according to claim 5, wherein the internal and external phase solutions are filled into two 10ml syringes, respectively, and the syringes are fixed to a syringe pump, and the solution amount and flow rate are set; connecting the microfluidic chip with a polyethylene tube; the microfluidic chip is fixed to be vertically placed, a collection culture dish is placed at the rear end of the microfluidic chip, and a calcium chloride solution is placed in the culture dish to serve as a collection liquid.

7. The method of claim 5, wherein the collection tube has an inner diameter of 1.0mm and a length of 65 mm; the maximum inner diameter of the injection tube is 300 mu m, the minimum inner diameter of the conical outlet is 80 mu m, and the length of the injection tube is 55 mm.

8. The method of claim 1, wherein the short length of the fiber is 1-2 cm.

9. The preparation method of claim 1, wherein the water bath heating temperature is 80-85 ℃ and the time is 2 h.

10. Medical dressing based on humifuse euphorbia herb extract prepared according to the preparation method of any one of the preceding claims.