CN110898087A - Electrostatic spinning substance, preparation method and application thereof, rheumatism patch and preparation method thereof - Google Patents
Electrostatic spinning substance, preparation method and application thereof, rheumatism patch and preparation method thereof Download PDFInfo
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Abstract
The invention discloses an electrostatic spinning substance, a preparation method and application thereof, a rheumatism patch and a preparation method thereof, and belongs to the technical field of medicines. The preparation method of the electrostatic spinning substance comprises the following steps: cutting up the liquidambar formosana mistletoe, and adding an ethanol water solution for extraction to obtain an extract liquid; sequentially carrying out evaporation concentration and vacuum freeze drying on the extract liquor, and carrying out supercritical extraction to obtain a supercritical extract of the liquidambar formosana mistletoe; performing supercritical extraction on the supercritical extract and lecithin to obtain an oil-phase solute; d-glucosamine hydrochloride aqueous solution is selected as aqueous phase solution, and after the aqueous phase solution is mixed with the oil phase dissolved substance, evaporation and concentration are carried out to obtain nano liposome extract; mixing the nano liposome extract with a gelatin solution to obtain a spinning solution; and (3) carrying out electrostatic spinning on the spinning solution to obtain the electrostatic spinning substance. The rheumatism plaster prepared by using the electrostatic spinning substance has the characteristics of long drug effect time, obvious curative effect and the like.
Description
Technical Field
The invention relates to the technical field of medicines, and particularly relates to an electrostatic spinning substance, a preparation method and application thereof, a rheumatism patch and a preparation method thereof.
Background
The occurrence of rheumatism is considered by traditional Chinese medicine that pathogenic factors of wind, cold and dampness are invaded into the body and are retained in meridians, tendons, bones or joints due to climate change, cold and heat alternation, or cold and dampness of the living part, or overstrain and trauma, so that qi and blood are blocked. For rheumatism, patients are mostly given nonsteroidal anti-inflammatory drugs, immunosuppressants, physical therapy, external drugs, intra-articular injection and the like in western medicine, the drugs can control the disease progress to a certain extent and slow down the bone destruction and the joint deformity, but the drugs have relatively more adverse effects. The traditional Chinese medicine obtains a certain effect on treating chronic rheumatic arthritis by syndrome differentiation.
In the prior art, the rheumatism plaster generally uses the traditional fiber cloth as a main component of the plaster, and is used in a form of the plaster, so that the preparation process is complex and tedious, and if the rheumatism plaster of the type needs to be used for a long time, a pasting part has great stimulation to skin, secondary damage is easy to generate, and the problem that effective components are not easy to absorb exists.
Disclosure of Invention
An object of the embodiments of the present invention is to provide a method for preparing an electrospun material, so as to solve the problems in the background art.
In order to achieve the above purpose, the embodiments of the present invention provide the following technical solutions:
a method of preparing an electrospun material comprising the steps of:
cutting up the whole plant of the liquidambar formosana mistletoe, and adding an ethanol water solution for extraction to obtain an extract liquid;
sequentially carrying out evaporation concentration and vacuum freeze drying on the extract liquor to obtain dry powder;
selecting ethanol and carbon dioxide as entrainers, and performing supercritical extraction on the dry powder to obtain a supercritical extract of the Liquidambar formosana mistletoe;
mixing the supercritical extract and lecithin according to the mass ratio of 1 (0.5-1.5), and performing supercritical extraction to obtain an oil phase dissolved substance;
d-glucosamine hydrochloride aqueous solution is selected as aqueous phase solution, and the aqueous phase solution and the oil phase dissolved substance are mixed by a spraying mode and then are evaporated and concentrated to obtain nano liposome extract;
mixing the nano liposome extract with a gelatin solution to obtain a spinning solution;
and (3) carrying out electrostatic spinning on the spinning solution to obtain the electrostatic spinning substance.
In the step of performing supercritical extraction on the dry powder by using ethanol and carbon dioxide as entrainers to obtain the supercritical extract of the Liquidambar formosana Hance, the temperature of the supercritical extraction is 50-70 ℃, and the pressure of the supercritical extraction is 35-55 MPa; in the supercritical extraction process, the flow rate of the ethanol is 0.5-1.5 mL/min, and the flow rate of the carbon dioxide is 4-6L/min.
In another preferable scheme of the embodiment of the invention, in the step of mixing the supercritical extract and the lecithin according to the mass ratio of 1 (0.5-1.5) and performing supercritical extraction to obtain the oil-phase dissolved substance, the temperature of the supercritical extraction is 50-70 ℃, and the pressure of the supercritical extraction is 13-17 MPa.
In another preferred embodiment of the present invention, in the step of mixing the aqueous phase solution and the oil phase dissolved substance by spraying, and then evaporating and concentrating to obtain the nanoliposome extract, the spraying pressure is 10 to 14MPa, and the temperature of the spray head used for spraying is 80 to 90 ℃.
In another preferable embodiment of the invention, in the step of obtaining the electrostatic spinning product by electrostatic spinning of the spinning solution, the feed rate of the spinning solution is 0.3 to 0.7mL/h, and the voltage applied in the electrostatic spinning process is 20 to 30 kV.
Another object of the embodiments of the present invention is to provide an electrospun material prepared by the above preparation method.
The embodiment of the invention also aims to provide application of the electrostatic spinning substance in preparing a medicine for treating rheumatism.
Another object of the embodiments of the present invention is to provide a rheumatism patch, which comprises the above electrostatic spinning material.
As another preferable scheme of the embodiment of the invention, the rheumatism patch comprises the following components in parts by weight: 1 to 30 parts of electrostatic spinning material, 0.025 to 0.4 part of chitosan, 0.025 to 0.4 part of borneol, 0.08 to 0.2 part of gelatin and 0.1 to 2 parts of glycerol.
Another object of the embodiments of the present invention is to provide a method for preparing the rheumatism patch, which comprises the following steps:
weighing the electrostatic spinning substance, chitosan, borneol, gelatin and glycerol according to the weight parts for later use;
dissolving chitosan in an aqueous solution with the pH value of 3-5 to obtain a chitosan aqueous solution; the mass concentration of chitosan in the chitosan aqueous solution is 0.5-2%;
dissolving Borneolum Syntheticum in ethanol to obtain Borneolum Syntheticum ethanol solution; the mass concentration of borneol in the borneol ethanol solution is 5-20 percent;
mixing gelatin with water to obtain gelatin solution; the mass concentration of gelatin in the gelatin solution is 1-2%;
mixing the chitosan water solution and the borneol ethanol solution, and then adding the electrostatic spinning substance and the glycerol for mixing to obtain the rheumatism patch.
The embodiment of the invention also aims to provide the rheumatism patch prepared by the preparation method.
Compared with the prior art, the embodiment of the invention has the beneficial effects that:
the electrostatic spinning substance prepared by the preparation method of the electrostatic spinning substance provided by the embodiment of the invention can be used for preparing medicines for treating rheumatism. The electrostatic spinning material is matched with components such as chitosan, borneol, gelatin, glycerol and the like to prepare the liquid nano rheumatism patch, and the rheumatism patch does not need a bandage of a rheumatism patch, can be directly used and can be completely degraded. By applying the rheumatism patch on the rheumatism affected part, the appearance is not affected and the movement of the body position is not limited by the application. Compared with the traditional rheumatism patch, the rheumatism patch provided by the invention adopts micro-nano-scale components, has a coating membrane structure similar to a human body cell membrane, has natural targeting property and good pore permeability, and is easy to permeate and absorb. In addition, as the effective components of D-glucosamine hydrochloride and the Liquidambar formosana Hance are effectively coated, the rheumatism patch has long effective time, long drug effect time and obvious curative effect on rheumatism.
Drawings
FIG. 1 is a fluorescence microscope image of nanoliposomes obtained in example 3 of the present invention.
FIG. 2 is a transmission electron microscope photograph of an electrospun obtained in example 3 of the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
The embodiment provides a preparation method of an electrostatic spinning substance and a rheumatism patch, wherein the preparation method of the electrostatic spinning substance comprises the following steps:
s1, chopping the whole plant of the Liquidambar formosana mistletoe, adding an equal amount of ethanol water solution, placing in a microwave extraction tank, and performing microwave extraction for 3min to obtain an extract.
And S2, evaporating and concentrating the extract by a rotary evaporation device, and then carrying out vacuum freeze drying to remove water to obtain dry powder.
S3, selecting ethanol and carbon dioxide as entrainers, placing the dry powder in a supercritical extraction kettle, performing supercritical extraction for 3h under the conditions that the temperature is 50 ℃, the pressure is 35MPa, the flow rate of the ethanol is 0.5mL/min and the flow rate of the carbon dioxide is 4L/min, and collecting the supercritical extract of the Liquidambar formosana mistletoe.
S4, mixing the supercritical extract and lecithin according to the mass ratio of 1:0.5, placing the mixture into a supercritical extraction kettle, performing supercritical extraction for 2 hours at the temperature of 50 ℃ and the pressure of 13MPa, and collecting oil phase dissolved substances (under the condition of supercritical carbon dioxide dissolution).
S5, dissolving D-glucosamine hydrochloride in pure water, preparing a saturated solution of the D-glucosamine hydrochloride at normal temperature, and filtering to remove undissolved solute to obtain a D-glucosamine hydrochloride aqueous solution; d-glucosamine hydrochloride aqueous solution is selected as aqueous phase solution, the aqueous phase solution and the oil phase dissolved substance are mixed in a spraying mode, and evaporation and concentration are carried out by a rotary evaporator to obtain nano liposome extract; the specific spraying method comprises the following steps: the size of a spray head connected with the high-pressure kettle is 0.5mm, the temperature of the spray head is 80 ℃, the pressure of the spray head is adjusted to be 10Mpa, the spray interval of the spray head is controlled to be 1s by an electromagnetic valve, and a stainless steel pipe with the diameter of 0.5mm is used for connecting the water phase solution in a spray head cavity and is vertically involuted with the spray head. In the process of spraying by a nozzle, the water phase solution is automatically mixed with the oil phase dissolved substance in the cavity due to the Bernoulli effect, so that the nano liposome with the core material of D-glucosamine hydrochloride and the wall material of phospholipid containing the effective components of the Liquidambar formosana Hance is obtained.
S6, mixing the nano liposome extract with a gelatin solution to obtain a spinning solution; the preparation method of the gelatin solution comprises the following steps: putting gelatin into appropriate amount of cold water, heating with hot water bath after gelatin absorbs water and swells, and stirring until gelatin solution is obtained.
And S7, placing the spinning solution in a nano electrostatic spinning machine for electrostatic spinning to obtain the electrostatic spinning substance. Wherein, the voltage between the spinning nozzle and the collecting plate of the nano electrostatic spinning machine is 20kV, the distance between the spinning nozzle and the collecting plate is 4cm, and the liquid inlet speed of the spinning solution is 0.3 mL/h.
In addition, the preparation method of the rheumatism patch comprises the following steps:
(1) weighing 10g of electrostatic spinning matter, 0.25g of chitosan, 0.25g of borneol, 0.8g of gelatin and 1g of glycerol for later use;
(2) dissolving chitosan in water solution with pH value of 3, and stirring for 30min to obtain chitosan water solution with chitosan mass concentration of 0.5%.
(3) Dissolving borneol in ethanol to prepare borneol ethanol solution with the mass concentration of the borneol of 5 percent.
(4) Mixing gelatin with water to obtain gelatin solution; specifically, gelatin is put into a proper amount of cold water, heated by a hot water bath after the gelatin absorbs water and expands, and stirred until the gelatin is dissolved, so as to prepare a gelatin solution with the gelatin mass concentration of 1%.
(5) Mixing the chitosan aqueous solution and the borneol ethanol solution, adding the electrostatic spinning substance and the glycerol for mixing, and stirring uniformly to obtain the liquid rheumatism plaster.
Example 2
The embodiment provides a preparation method of an electrostatic spinning substance and a rheumatism patch, wherein the preparation method of the electrostatic spinning substance comprises the following steps:
s1, chopping the whole plant of the Liquidambar formosana mistletoe, adding an equal amount of ethanol water solution, placing in a microwave extraction tank, and performing microwave extraction for 5min to obtain an extract.
And S2, evaporating and concentrating the extract by a rotary evaporation device, and then carrying out vacuum freeze drying to remove water to obtain dry powder.
S3, selecting ethanol and carbon dioxide as entrainers, placing the dry powder in a supercritical extraction kettle, performing supercritical extraction for 3h under the conditions that the temperature is 70 ℃, the pressure is 55MPa, the flow rate of the ethanol is 1.5mL/min and the flow rate of the carbon dioxide is 6L/min, and collecting the supercritical extract of the Liquidambar formosana mistletoe.
S4, mixing the supercritical extract and lecithin according to the mass ratio of 1:1.5, placing the mixture into a supercritical extraction kettle, performing supercritical extraction for 2 hours at the temperature of 70 ℃ and the pressure of 17MPa, and collecting oil phase dissolved substances (under the condition of supercritical carbon dioxide dissolution).
S5, dissolving D-glucosamine hydrochloride in pure water, preparing a saturated solution of the D-glucosamine hydrochloride at normal temperature, and filtering to remove undissolved solute to obtain a D-glucosamine hydrochloride aqueous solution; d-glucosamine hydrochloride aqueous solution is selected as aqueous phase solution, the aqueous phase solution and the oil phase dissolved substance are mixed in a spraying mode, and evaporation and concentration are carried out by a rotary evaporator to obtain nano liposome extract; the specific spraying method comprises the following steps: the size of a spray head connected with the high-pressure kettle is 1.5mm, the temperature of the spray head is 90 ℃, the pressure of the spray head is adjusted to be 14Mpa, the spray interval of the spray head is controlled to be 1s by using an electromagnetic valve, and a stainless steel pipe with the diameter of 0.5mm is used for connecting the aqueous phase solution in a spray head cavity and vertically involuting with the spray head. In the process of spraying by a nozzle, the water phase solution is automatically mixed with the oil phase dissolved substance in the cavity due to the Bernoulli effect, so that the nano liposome with the core material of D-glucosamine hydrochloride and the wall material of phospholipid containing the effective components of the Liquidambar formosana Hance is obtained.
S6, mixing the nano liposome extract with a gelatin solution to obtain a spinning solution; the preparation method of the gelatin solution comprises the following steps: putting gelatin into appropriate amount of cold water, heating with hot water bath after gelatin absorbs water and swells, and stirring until gelatin solution is obtained.
And S7, placing the spinning solution in a nano electrostatic spinning machine for electrostatic spinning to obtain the electrostatic spinning substance. Wherein, the voltage between the spinning nozzle and the collecting plate of the nano electrostatic spinning machine is 30kV, the distance between the spinning nozzle and the collecting plate is 6cm, and the liquid inlet speed of the spinning solution is 0.7 mL/h.
In addition, the preparation method of the rheumatism patch comprises the following steps:
(1) weighing 300g of electrostatic spinning matter, 4g of chitosan, 4g of borneol, 2g of gelatin and 20g of glycerol for later use;
(2) dissolving chitosan in water solution with pH value of 5, and stirring for 30min to prepare chitosan water solution with chitosan mass concentration of 2%.
(3) Dissolving Borneolum Syntheticum in ethanol to obtain Borneolum Syntheticum ethanol solution with Borneolum Syntheticum mass concentration of 20%.
(4) Mixing gelatin with water to obtain gelatin solution; specifically, gelatin is put into a proper amount of cold water, heated by a hot water bath after the gelatin absorbs water and expands, and stirred until the gelatin is dissolved, so as to prepare a gelatin solution with the gelatin mass concentration of 2%.
(5) Mixing the chitosan aqueous solution and the borneol ethanol solution, adding the electrostatic spinning substance and the glycerol for mixing, and stirring uniformly to obtain the liquid rheumatism plaster.
Example 3
The embodiment provides a preparation method of an electrostatic spinning substance and a rheumatism patch, wherein the preparation method of the electrostatic spinning substance comprises the following steps:
s1, chopping the whole plant of the Liquidambar formosana mistletoe, adding an equal amount of ethanol water solution, placing in a microwave extraction tank, and performing microwave extraction for 4min to obtain an extract.
And S2, evaporating and concentrating the extract by a rotary evaporation device, and then carrying out vacuum freeze drying to remove water to obtain dry powder.
S3, selecting ethanol and carbon dioxide as entrainers, placing the dry powder in a supercritical extraction kettle, performing supercritical extraction for 3 hours at the temperature of 50-60 ℃, the pressure of 45MPa, the flow rate of the ethanol of 1mL/min and the flow rate of the carbon dioxide of 5L/min, and collecting to obtain the supercritical extract of the Liquidambar formosana mistletoe.
S4, mixing the supercritical extract and lecithin according to the mass ratio of 1:1, placing the mixture into a supercritical extraction kettle, performing supercritical extraction for 2 hours at the temperature of 60 ℃ and the pressure of 15MPa, and collecting oil phase dissolved substances (under the condition of supercritical carbon dioxide dissolution).
S5, dissolving D-glucosamine hydrochloride in pure water, preparing a saturated solution of the D-glucosamine hydrochloride at normal temperature, and filtering to remove undissolved solute to obtain a D-glucosamine hydrochloride aqueous solution; d-glucosamine hydrochloride aqueous solution is selected as aqueous phase solution, the aqueous phase solution and the oil phase dissolved substance are mixed in a spraying mode, and evaporation and concentration are carried out by a rotary evaporator to obtain nano liposome extract; the specific spraying method comprises the following steps: the size of a spray head connected with the high-pressure kettle is 1mm, the temperature of the spray head is 90 ℃, the pressure of the spray head is adjusted to be 12Mpa, the spray interval of the spray head is controlled to be 1s by using an electromagnetic valve, and a stainless steel pipe with the diameter of 0.5mm is used for connecting the water phase solution in a spray head cavity and is vertically involuted with the spray head. In the process of spraying by a nozzle, due to Bernoulli effect, the aqueous phase solution is automatically mixed with the oil phase dissolved substance in the cavity, so that the nano liposome with the core material of D-glucosamine hydrochloride and the wall material of phospholipid containing the effective component of Dendropanax formosanus can be obtained, and the fluorescence microscopy (PR300 type, Shanghai Pan' er photoelectric instrument) diagram of the nano liposome is shown as the attached figure 1.
S6, mixing the nano liposome extract with a gelatin solution to obtain a spinning solution; the preparation method of the gelatin solution comprises the following steps: putting gelatin into appropriate amount of cold water, heating with hot water bath after gelatin absorbs water and swells, and stirring until gelatin solution is obtained.
S7, placing the spinning solution in a nano electrostatic spinning machine for electrostatic spinning to obtain the electrostatic spinning substance, wherein the transmission electron microscope (JEM-2100Plus) picture of the electrostatic spinning substance is shown as the attached figure 2. Wherein, the voltage between the spinning nozzle and the collecting plate of the nano electrostatic spinning machine is 25kV, the distance between the spinning nozzle and the collecting plate is 5cm, and the liquid inlet speed of the spinning solution is 0.5 mL/h.
In addition, the preparation method of the rheumatism patch comprises the following steps:
(1) weighing 150g of electrostatic spinning matter, 1g of chitosan, 1g of borneol, 1.35g of gelatin and 7.14g of glycerol for later use;
(2) dissolving chitosan in the aqueous solution with the pH value of 4, and stirring for 30min to prepare the chitosan aqueous solution with the mass concentration of chitosan of 1%.
(3) Dissolving Borneolum Syntheticum in ethanol to obtain Borneolum Syntheticum ethanol solution with Borneolum Syntheticum mass concentration of 10%.
(4) Mixing gelatin with water to obtain gelatin solution; specifically, gelatin is put into a proper amount of cold water, heated by a hot water bath after the gelatin absorbs water and expands, and stirred until the gelatin is dissolved, so as to prepare a gelatin solution with the gelatin mass concentration of 1.5%.
(5) Mixing the chitosan aqueous solution and the borneol ethanol solution, adding the electrostatic spinning substance and the glycerol for mixing, and stirring uniformly to obtain the liquid rheumatism plaster.
Example 4
The embodiment provides a preparation method of an electrostatic spinning substance and a rheumatism patch, wherein the preparation method of the electrostatic spinning substance comprises the following steps:
s1, chopping the whole plant of the Liquidambar formosana mistletoe, adding an equal amount of ethanol water solution, placing in a microwave extraction tank, and performing microwave extraction for 3min to obtain an extract.
And S2, evaporating and concentrating the extract by a rotary evaporation device, and then carrying out vacuum freeze drying to remove water to obtain dry powder.
S3, selecting ethanol and carbon dioxide as entrainers, placing the dry powder in a supercritical extraction kettle, performing supercritical extraction for 3 hours at the temperature of 50-60 ℃, the pressure of 45MPa, the flow rate of the ethanol of 1mL/min and the flow rate of the carbon dioxide of 5L/min, and collecting to obtain the supercritical extract of the Liquidambar formosana mistletoe.
S4, mixing the supercritical extract and lecithin according to the mass ratio of 1:1, placing the mixture into a supercritical extraction kettle, performing supercritical extraction for 2 hours at the temperature of 60 ℃ and the pressure of 13.5MPa, and collecting oil phase dissolved substances (under the condition of supercritical carbon dioxide dissolution).
S5, dissolving D-glucosamine hydrochloride in pure water, preparing a saturated solution of the D-glucosamine hydrochloride at normal temperature, and filtering to remove undissolved solute to obtain a D-glucosamine hydrochloride aqueous solution; d-glucosamine hydrochloride aqueous solution is selected as aqueous phase solution, the aqueous phase solution and the oil phase dissolved substance are mixed in a spraying mode, and evaporation and concentration are carried out by a rotary evaporator to obtain nano liposome extract; the specific spraying method comprises the following steps: the size of a spray head connected with the high-pressure kettle is 0.5mm, the temperature of the spray head is 90 ℃, the pressure of the spray head is adjusted to be 10Mpa, the spray interval of the spray head is controlled to be 1s by an electromagnetic valve, and a stainless steel pipe with the diameter of 0.5mm is used for connecting the water phase solution in a spray head cavity and vertically involuting with the spray head. In the process of spraying by a nozzle, the water phase solution is automatically mixed with the oil phase dissolved substance in the cavity due to the Bernoulli effect, so that the nano liposome with the core material of D-glucosamine hydrochloride and the wall material of phospholipid containing the effective components of the Liquidambar formosana Hance is obtained.
S6, mixing the nano liposome extract with a gelatin solution to obtain a spinning solution; the preparation method of the gelatin solution comprises the following steps: putting gelatin into appropriate amount of cold water, heating with hot water bath after gelatin absorbs water and swells, and stirring until gelatin solution is obtained.
And S7, placing the spinning solution in a nano electrostatic spinning machine for electrostatic spinning to obtain the electrostatic spinning substance. Wherein, the voltage between the spinning nozzle and the collecting plate of the nano electrostatic spinning machine is 25kV, the distance between the spinning nozzle and the collecting plate is 5cm, and the liquid inlet speed of the spinning solution is 0.5 mL/h.
In addition, the preparation method of the rheumatism patch comprises the following steps:
(1) weighing 300g of electrostatic spinning matter, 1.8g of chitosan, 3g of borneol, 0.8g of gelatin and 5.85g of glycerol for later use;
(2) dissolving chitosan in water solution with pH value of 3, and stirring for 30min to prepare chitosan water solution with chitosan mass concentration of 1%.
(3) Dissolving borneol in ethanol to prepare a borneol ethanol solution with the mass concentration of the borneol of 15 percent.
(4) Mixing gelatin with water to obtain gelatin solution; specifically, gelatin is put into a proper amount of cold water, heated by a hot water bath after the gelatin absorbs water and expands, and stirred until the gelatin is dissolved, so as to prepare a gelatin solution with the gelatin mass concentration of 1%.
(5) Mixing the chitosan aqueous solution and the borneol ethanol solution, adding the electrostatic spinning substance and the glycerol for mixing, and stirring uniformly to obtain the liquid rheumatism plaster.
Example 5
The embodiment provides a preparation method of an electrostatic spinning substance and a rheumatism patch, wherein the preparation method of the electrostatic spinning substance comprises the following steps:
s1, chopping the whole plant of the Liquidambar formosana mistletoe, adding an equal amount of ethanol water solution, placing in a microwave extraction tank, and performing microwave extraction for 4min to obtain an extract.
And S2, evaporating and concentrating the extract by a rotary evaporation device, and then carrying out vacuum freeze drying to remove water to obtain dry powder.
S3, selecting ethanol and carbon dioxide as entrainers, placing the dry powder in a supercritical extraction kettle, performing supercritical extraction for 3 hours at the temperature of 50-60 ℃, the pressure of 45MPa, the flow rate of the ethanol of 1mL/min and the flow rate of the carbon dioxide of 5L/min, and collecting to obtain the supercritical extract of the Liquidambar formosana mistletoe.
S4, mixing the supercritical extract and lecithin according to the mass ratio of 1:1, placing the mixture into a supercritical extraction kettle, performing supercritical extraction for 2 hours at the temperature of 60 ℃ and under the pressure of 16MPa, and collecting oil phase dissolved substances (under the condition of supercritical carbon dioxide dissolution).
S5, dissolving D-glucosamine hydrochloride in pure water, preparing a saturated solution of the D-glucosamine hydrochloride at normal temperature, and filtering to remove undissolved solute to obtain a D-glucosamine hydrochloride aqueous solution; d-glucosamine hydrochloride aqueous solution is selected as aqueous phase solution, the aqueous phase solution and the oil phase dissolved substance are mixed in a spraying mode, and evaporation and concentration are carried out by a rotary evaporator to obtain nano liposome extract; the specific spraying method comprises the following steps: the size of a spray head connected with the high-pressure kettle is 1mm, the temperature of the spray head is 90 ℃, the pressure of the spray head is adjusted to be 11Mpa, the spray interval of the spray head is controlled to be 1s by using an electromagnetic valve, and a stainless steel pipe with the diameter of 0.5mm is used for connecting the water phase solution in a spray head cavity and vertically involuting with the spray head. In the process of spraying by a nozzle, the water phase solution is automatically mixed with the oil phase dissolved substance in the cavity due to the Bernoulli effect, so that the nano liposome with the core material of D-glucosamine hydrochloride and the wall material of phospholipid containing the effective components of the Liquidambar formosana Hance is obtained.
S6, mixing the nano liposome extract with a gelatin solution to obtain a spinning solution; the preparation method of the gelatin solution comprises the following steps: putting gelatin into appropriate amount of cold water, heating with hot water bath after gelatin absorbs water and swells, and stirring until gelatin solution is obtained.
And S7, placing the spinning solution in a nano electrostatic spinning machine for electrostatic spinning to obtain the electrostatic spinning substance. Wherein, the voltage between the spinning nozzle and the collecting plate of the nano electrostatic spinning machine is 25kV, the distance between the spinning nozzle and the collecting plate is 5c m, and the liquid inlet speed of the spinning solution is 0.5 mL/h.
In addition, the preparation method of the rheumatism patch comprises the following steps:
(1) weighing 280g of electrostatic spinning product, 3.61g of chitosan, 0.55g of borneol, 0.8g of gelatin and 11.4g of glycerol for later use;
(2) dissolving chitosan in water solution with pH value of 3.5, and stirring for 30min to obtain chitosan water solution with chitosan mass concentration of 1.9%.
(3) Dissolving Borneolum Syntheticum in ethanol to obtain Borneolum Syntheticum ethanol solution with Borneolum Syntheticum mass concentration of 5.5%.
(4) Mixing gelatin with water to obtain gelatin solution; specifically, gelatin is put into a proper amount of cold water, heated by a hot water bath after the gelatin absorbs water and expands, and stirred until the gelatin is dissolved, so as to prepare a gelatin solution with the gelatin mass concentration of 1%.
(5) Mixing the chitosan aqueous solution and the borneol ethanol solution, adding the electrostatic spinning substance and the glycerol for mixing, and stirring uniformly to obtain the liquid rheumatism plaster.
In the embodiment of the present invention, 30 volunteers used the rheumatism patch prepared by the preparation method provided in the above embodiment 3, and the film forming effect, self-feeling condition and treatment effect of the rheumatism patch after use were scored according to the use conditions, and the scoring results are shown in table 1. The application method of the rheumatism patch comprises the following steps: directly and uniformly applying the rheumatism patch on the affected part; in addition, the reference criteria for each score are as follows:
the rheumatism plaster has the film forming effect: the rheumatism plaster does not form a film for-1 min, the rheumatism plaster does not completely form a film for-2 min, and the rheumatism plaster completely forms a film for-3 min;
self-feeling condition of the patient: the effect is very obvious, namely, the effect is as good as-1 point and-2 points, the effect is as good as-3 points, and no feeling is given as-4 points;
the treatment effect is as follows: the curative effect is obvious for-1 point, the curative effect is good for-2 points, the curative effect is-3 points, the curative effect is general for-4 points, and the curative effect is not-5 points.
The final score values are expressed as mean ± standard error (N ═ 30).
TABLE 1
| Scoring item | Applying for 1min | Smearing for 3min | Smearing for 5min | After being smeared for 1 hour | After being smeared for 1d | After being coated for 2d |
| Film forming effect of rheumatism plaster | 2.20±0.41 | 2.93±0.25 | 3±0 | 3±0 | - | - |
| Patient self-feeling condition | - | - | 2.80±0.89 | - | - | 1.70±0.79 |
| Therapeutic effects | - | - | - | 2.10±0.31 | - | 1.53±0.68 |
As can be seen from the above table 1, the rheumatism plaster prepared by the embodiment of the invention can be directly smeared on affected parts, and has the advantages of fast film formation, fast curative effect and better curative effect.
In light of the foregoing description of the preferred embodiment of the present invention, many modifications and variations will be apparent to those skilled in the art without departing from the spirit and scope of the invention. The technical scope of the present invention is not limited to the content of the specification, and must be determined according to the scope of the claims.
Claims (10)
1. A method for preparing an electrospun, comprising the steps of:
cutting up the whole plant of the liquidambar formosana mistletoe, and adding an ethanol water solution for extraction to obtain an extract liquid;
sequentially carrying out evaporation concentration and vacuum freeze drying on the extract liquor to obtain dry powder;
selecting ethanol and carbon dioxide as entrainers, and performing supercritical extraction on the dry powder to obtain a supercritical extract of the Liquidambar formosana mistletoe;
mixing the supercritical extract and lecithin according to the mass ratio of 1 (0.5-1.5), and performing supercritical extraction to obtain an oil phase dissolved substance;
d-glucosamine hydrochloride aqueous solution is selected as aqueous phase solution, and the aqueous phase solution and the oil phase dissolved substance are mixed by a spraying mode and then are evaporated and concentrated to obtain nano liposome extract;
mixing the nano liposome extract with a gelatin solution to obtain a spinning solution;
and (3) carrying out electrostatic spinning on the spinning solution to obtain the electrostatic spinning substance.
2. The method for preparing the electrostatic spinning substance according to claim 1, wherein in the step of performing supercritical extraction on the dry powder by using ethanol and carbon dioxide as entrainers to obtain the supercritical extract of the Viscum album, the temperature of the supercritical extraction is 50-70 ℃, and the pressure of the supercritical extraction is 35-55 MPa; in the supercritical extraction process, the flow rate of the ethanol is 0.5-1.5 mL/min, and the flow rate of the carbon dioxide is 4-6L/min.
3. The method for preparing an electrospun according to claim 1, wherein in the step of mixing the supercritical extract with lecithin in a mass ratio of 1 (0.5-1.5) and performing supercritical extraction to obtain the oil-phase solute, the temperature of the supercritical extraction is 50-70 ℃, and the pressure of the supercritical extraction is 13-17 MPa.
4. The method of claim 1, wherein in the step of electrospinning the spinning solution to obtain the electrospun material, the feed rate of the spinning solution is 0.3 to 0.7mL/h, and the voltage applied during electrospinning is 20 to 30 kV.
5. An electrospun product obtainable by the process according to any one of claims 1 to 4.
6. Use of the electrospun of claim 5 in the preparation of a medicament for the treatment of rheumatism.
7. A rheumatism patch characterized by comprising the electrospun substance of claim 5.
8. The rheumatism patch as claimed in claim 7, which is characterized by comprising the following components in parts by weight: 1 to 30 parts of electrostatic spinning material, 0.025 to 0.4 part of chitosan, 0.025 to 0.4 part of borneol, 0.08 to 0.2 part of gelatin and 0.1 to 2 parts of glycerol.
9. The preparation method of the rheumatism patch as claimed in claim 8, which comprises the following steps:
weighing the electrostatic spinning substance, chitosan, borneol, gelatin and glycerol according to the weight parts for later use;
dissolving chitosan in an aqueous solution with the pH value of 3-5 to obtain a chitosan aqueous solution; the mass concentration of chitosan in the chitosan aqueous solution is 0.5-2%;
dissolving Borneolum Syntheticum in ethanol to obtain Borneolum Syntheticum ethanol solution; the mass concentration of borneol in the borneol ethanol solution is 5-20 percent;
mixing gelatin with water to obtain gelatin solution; the mass concentration of gelatin in the gelatin solution is 1-2%;
mixing the chitosan water solution and the borneol ethanol solution, and then adding the electrostatic spinning substance and the glycerol for mixing to obtain the rheumatism patch.
10. A rheumatism patch prepared by the preparation method of claim 9.
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