CN106801261B - A kind of electro spinning nano fiber and preparation method thereof with drug gradient distribution - Google Patents
A kind of electro spinning nano fiber and preparation method thereof with drug gradient distribution Download PDFInfo
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- CN106801261B CN106801261B CN201710010815.1A CN201710010815A CN106801261B CN 106801261 B CN106801261 B CN 106801261B CN 201710010815 A CN201710010815 A CN 201710010815A CN 106801261 B CN106801261 B CN 106801261B
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- fluid injector
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/0007—Electro-spinning
- D01D5/0061—Electro-spinning characterised by the electro-spinning apparatus
- D01D5/0069—Electro-spinning characterised by the electro-spinning apparatus characterised by the spinning section, e.g. capillary tube, protrusion or pin
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/28—Formation of filaments, threads, or the like while mixing different spinning solutions or melts during the spinning operation; Spinnerette packs therefor
- D01D5/30—Conjugate filaments; Spinnerette packs therefor
- D01D5/34—Core-skin structure; Spinnerette packs therefor
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/10—Other agents for modifying properties
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F2/00—Monocomponent artificial filaments or the like of cellulose or cellulose derivatives; Manufacture thereof
- D01F2/24—Monocomponent artificial filaments or the like of cellulose or cellulose derivatives; Manufacture thereof from cellulose derivatives
- D01F2/28—Monocomponent artificial filaments or the like of cellulose or cellulose derivatives; Manufacture thereof from cellulose derivatives from organic cellulose esters or ethers, e.g. cellulose acetate
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- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Mechanical Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Manufacturing & Machinery (AREA)
- Spinning Methods And Devices For Manufacturing Artificial Fibers (AREA)
Abstract
The present invention provides a kind of medicament-carrying nano-fibers with drug gradient distribution, including an inner sandwich layer, the periphery of the inner sandwich layer is provided with middle layer, the periphery of the middle layer is provided with extexine, inner sandwich layer, middle layer and the extexine coaxially extends, contain drug in the inner sandwich layer, middle layer and extexine, concentration in gradient successively increases the drug from outside to inside.The present invention also provides the preparation methods of the above-mentioned nanofiber with drug gradient distribution.Additionally provide the device for realizing the above method.Method preparation process of the invention is simple, and single step is effective, in the nanofiber of preparation/in/outer three-decker is clear, and nanometer diameter is small, good linearity, diameter are evenly distributed, and fiber surface is smooth.The drug gradient distribution can provide effective for designing and preparing for numerous sustained and controlled release medicine materials.
Description
Technical field
The invention belongs to materialogy fields, are related to a kind of structure-activity relationship establishing techniques of novel nano level substance, specifically
For be a kind of electro spinning nano fiber and preparation method thereof with drug gradient distribution.
Background technique
High-voltage electrostatic spinning technology (electrospinning) is the nano-fabrication technique of a kind of (top-down) from top to bottom, by additional
The jet stream that electric field force overcomes the surface tension of liquid of spray head tip drop and viscoelastic power to be formed, in electrostatic repulsion, Coulomb force and table
Under the tension collective effect of face, the liquid jet after being atomized is drafted thousand by high frequency flexural, drawing, division within a few tens of milliseconds
Wan Bei obtains nano-scale fiber in receiving end after solvent volatilization or melt are cooling.The technical matters process is simple, manipulation side
Just, selection material ranges are extensive, controllability is strong, are considered as most possible one kind for realizing continuous nano-fibre industrialized production
Method prepares functional nano-fiber with good prospect using the technology.
Electric spinning polymer functional nano-fiber is assigned by addition active constituent and being received generally using fibre-forming polymer as substrate
Rice fiber function, and make full use of the special performance of electro spinning nanometer fiber membrane and give full play to the effectiveness of active constituent.These are solely
Special performance includes that fibre diameter is small, fiber surface area is big, fiber has in three-dimensional netted porous structure, porosity height, fiber
The diameter of nanoscale range but has the length etc. of macro-scope simultaneously.In biomedicine field, generally drug is added poly-
Polymer solution forms solution altogether and passes through the rapid draing and molding of common electro-spinning process, acquisition medicaments uniformity as spinning solution
It is distributed in the medicament-carrying nano-fiber of entire nanofiber.Most medicament-carrying nano-fibers are all the distributions of such medicaments uniformity and tie
The single nanofiber of structure obtains required drug by the characteristics of physicochemical property and nano fibrous membrane of polymeric substrate
Slow controlled release properties.Though having on a small quantity by the distribution of coaxial electrically spun and electrospinning regulating medicine arranged side by side in nanofiber, to obtain
Need the electrospinning core sheath nanofiber and Qiao Nasi nanofiber of medicine controlled releasing performance, but the nano junction about other structures feature
The preparation of structure and these structures are applied in terms of the controlled release properties for providing drug to be seldom reported.
Summary of the invention
For above-mentioned technical problem in the prior art, the present invention provides a kind of electricity with drug gradient distribution
Spinning nano fibre and preparation method thereof, this electro spinning nano fiber and its preparation side with drug gradient distribution
Method will solve the bad technical problem of medicine sustained and controlled release performance in the prior art.
The present invention provides a kind of medicament-carrying nano-fiber with drug gradient distribution, including an inner sandwich layer, institutes
The periphery for the inner sandwich layer stated is provided with middle layer, and the periphery of the middle layer is provided with extexine, the inner sandwich layer, centre
Layer and extexine coaxially extend, and contain drug in the inner sandwich layer, middle layer and extexine, and the drug is by outside extremely
Interior concentration in gradient successively increases.
The present invention also provides a kind of above-mentioned medicament-carrying nano-fibers with drug gradient distribution, including walk as follows
It is rapid:
1) mother liquor is made into using spinnable polymer solution, and the mother liquor after preparing is divided into first part's mother liquor, second
Partial mother liquid and Part III mother liquor；
2) add in first part's mother liquor, second part mother liquor and Part III mother liquor according to the increased sequence of concentration gradient
Enter drug, stir evenly, sequentially forms extexine working fluid, middle layer working fluid, inner sandwich layer working fluid, and corresponding dress
Enter extexine fluid injector, middle layer fluid injector, in inner sandwich layer fluid injector, the extexine fluid injector
One end connected with an appearance layer fluid syringe pump, the intermediate layer fluid of one end of the middle layer fluid injector and one
Syringe pump connection, one end of the inner sandwich layer fluid injector is connected with an inner core layer fluid syringe pump, using one three
The coaxial spinneret of grade, the coaxial spinneret of the three-level includes the coaxial capillary of internal layer, the coaxial capillary in middle layer, the coaxial hair of outer layer
The inside of coaxial capillary in middle level, the coaxial capillary setting in the middle layer is arranged in tubule, the coaxial capillary of the internal layer
In the inside of the coaxial capillary of outer layer, the extexine fluid injector is connected with the coaxial capillary of the outer layer, described
Middle layer fluid injector connected with the coaxial capillary in the middle layer, the inner sandwich layer fluid injector and described interior
The coaxial capillary connection of layer, opens high pressure generator, controls three laminar flows in the coaxial spinneret of three-level respectively by three syringe pumps
The injection rate of body, using the coaxial spinneret exit orifices of three-level as template, is prepared with drug gradient under the action of high-pressure electrostatic
The nanofiber of distribution characteristics, and plate is received by fiber and is received.
The present invention also provides the three-level coaxial electrically spun device for realizing the above method, an including coaxial spinneret of three-level,
The coaxial spinneret of the three-level includes the coaxial capillary of internal layer, the coaxial capillary in middle layer, the coaxial capillary of outer layer, and described is interior
The inside of coaxial capillary in middle level is arranged in the coaxial capillary of layer, and the coaxial capillary in the middle layer is arranged in the coaxial capillary of outer layer
The inside of pipe；It further include extexine fluid injector, middle layer fluid injector, inner sandwich layer fluid injector, the appearance
One end of layer fluid syringe is connected with an appearance layer fluid syringe pump, one end and one of the middle layer fluid injector
A intermediate layer fluid syringe pump connection, one end of the inner sandwich layer fluid injector and an inner core layer fluid syringe pump connect
Connect, the extexine fluid injector is connected with the coaxial capillary of the outer layer, the middle layer fluid injector and
The coaxial capillary connection in the middle layer, the inner sandwich layer fluid injector are connected with the coaxial capillary of the internal layer；Also
Including a high pressure generator, the high pressure generator is connected with the coaxial spinneret of the three-level, and the three-level is coaxial
The lower end of the outlet of spinneret is provided with fiber and receives plate.
Further, it is coaxial with three-level to pass through high resiliency silica gel hose for the inner sandwich layer and middle layer fluid injector
Internal layer capillary in spinneret is connected with middle layer capillary.
Nanofiber of the invention by inside and outside package three-level core sheath structure feature；Fibrous inside drug distribution gradient；
The Gradient Features refer to from outer layer that by middle layer, the mode that drug delivery adds is sequentially increased to internal layer；The structural fibers can be with
Effectively implement to prepare using three-level coaxial electrically spun technique single step, and is capable of providing the Zero order controlled releasing effect of drug.
The present invention is compared with prior art, and technological progress is significant.The present invention is that one kind passes through drug in the fibre
Gradient distribution obtain needed for drug Zero order controlled releasing performance electro spinning nano fiber.Method preparation process of the invention is simple, single
Step effectively, in the nanofiber of preparation/in/outer three-decker is clear and nanometer diameter is small, good linearity, diameter are evenly distributed,
Fiber surface is smooth.The drug gradient distribution can provide effective reality for designing and preparing for numerous sustained and controlled release medicine materials
Applying method.
Detailed description of the invention
Fig. 1 is the Taylor cone observation figure that the coaxial technique of three-level that the present invention uses prepares nanofiber.
Fig. 2 three-level coaxial electrically spun technology implementation schematic diagram.1- high pressure generator；The outer layer fluid syringe pump of 2-；In 3-
Between fluid syringe pump；4- internal layer fluid syringe pump；The coaxial spinneret of 5- three-level；6- fiber receiver sheet；7- high resiliency silica gel hose；
8- outer layer fluid injector；9- central fluid syringe；10- internal layer fluid injector.
Fig. 3 is the scanning electron microscope diagram with drug gradient distribution nanofiber of the invention.
Fig. 4 is the transmission electron microscope figure with drug gradient distribution nanofiber of the invention.
Fig. 5 is the structural schematic diagram that the present invention has drug gradient distribution nanofiber.
Fig. 6 is drug Zero order controlled releasing figure provided by nanofiber of the invention.
Specific embodiment
Below in conjunction with drawings and examples, the present invention is described in detail.These the examples are only for explaining the invention and
It is not intended to the limitation present invention.All uses and the same or similar method of the present invention, or the equivalent modifications made, should all fall into this
Invention protection scope.
Embodiment 1: the implementation of three-level coaxial electrically spun technique
36 grams of vinyl acetate celluloses are put into 300 grams to be made of acetone and N,N-dimethylformamide 3:1 in mass ratio
In the mixed solvent, be made into the mother liquor with favorable spinning quality.Above-mentioned mother liquor is divided into three parts, is added respectively wherein
Enter 1 gram, 3 grams and 5 grams of drug chlorphenamine maleate, through being stirred into it is transparent altogether solution, serve as internal layer, in
The working fluid of interbed and outer layer.By above-mentioned three kinds of working fluids be respectively charged into the inner sandwich layer of three-level coaxial electrically spun, middle layer and
In the syringe 10,9,8 of extexine working fluid, each layer fluid is connected into the coaxial spinneret 5 of three-level, connects high-pressure spinning head
With HV generator 1.According to following technological parameter implementation three-level coaxial high pressure electrostatic spinning process: internal layer/centre/
Outer layer fluid flow is 0.8/0.8/0.8 mL/h, and receiver board is 20 cm, 14 kV of voltage with a distance from spinning nozzle.Environment temperature
For (21 ± 3) DEG C, ambient humidity is 61 ± 5 %.In the above operating condition, bust shot in situ, electricity are carried out to electro-spinning process
Spinning process as shown in Figure 1, from the coaxial spinneret of three-level come out three-layer fluid a compound Taylor cone is collectively formed, cone
Top issues a straight jet, and straight jet is followed by the unstable region of high frequency stretching.Prepared nanofiber passes through
The aluminium foil package cardboard of one ground connection is collected.
Realize the three-level coaxial electrically spun device (such as Fig. 2) of the above method, including the coaxial spinneret 5 of a three-level, it is described
The coaxial spinneret 5 of three-level is made of internal layer capillary, middle layer capillary and the coaxial capillary of outer layer；It further include an inner sandwich layer
Fluid injector 10, middle layer fluid injector 9 and an extexine fluid injector 8；The inner sandwich layer fluid injector
10 one end and an inner core layer fluid syringe pump 4 connect, one end of middle layer fluid injector 9 and an intermediate layer fluid note
3 connection of pump is penetrated, one end of outer layer fluid injector 8 and an outer layer fluid syringe pump 2 connect, the inner core layer fluid injection
The other end of device 10 is connected with the coaxial capillary of the internal layer, the other end of middle layer fluid injector 9 and described
The coaxial capillary in middle layer connects, and the coaxial capillary connection of outer layer described in the other end of extexine fluid injector 8 further includes
One high pressure generator 1, the high pressure generator 1 and the coaxial spinneret 5 of the three-level connect, and the three-level is coaxially spun
The lower end that silk head 5 exports is arranged the fiber that the hardboard that useful Aluminium Foil Package is wrapped up in is made into and receives plate 6.
Further, the inner sandwich layer and middle layer fluid injector 10,9 pass through high resiliency silica gel hose and three-level
Internal layer capillary in coaxial spinneret 5 is connected with middle layer capillary.
Embodiment 2: the phenetic analysis with drug gradient distribution nanofiber pattern and structure
It is observed after carrying out surface metal spraying to fiber prepared by embodiment 1 using field emission scanning electron microscope (FESEM), as a result such as
Shown in Fig. 3.Good linear condition is presented in prepared fiber, does not have that bead structure, fiber surface be smooth, fiber accumulations
Uniformly.Diameter is 640 ± 130 nm, and distribution is relatively uniform, and concentration is compared in diameter distribution.
Prepared fibrous inner structure is observed using high resolution transmission electron microscopy (TEM), as a result such as Fig. 4 institute
Show, nanofiber it is interior/in/outer three-decker is clear, wherein outer layer is since medicament contg is few and thickness is thin, thus present compared with
Low gray scale, internal layer medicament contg is big, and thickness is big, therefore biggish gray scale is presented.
As shown in figure 5, a kind of medicament-carrying nano-fiber with drug gradient distribution is inner sandwich layer 11, centre
The three-level core sheath structure for the inside and outside package that layer 22 and extexine 33 are constituted, wherein from extexine 33 by middle layer 33 to inner core
Layer 22, the content of drug molecule 44 increases distribution in gradient.
Embodiment 3: there is brufen provided by drug gradient distribution nanofiber to delay controlled release properties
By 2015 editions annex of Chinese Pharmacopoeia, Ⅹ D drug release determination the second method slurry processes, experiment instrument is intelligently dissolved out using RCZ-8A
In Vitro Dissolution test is carried out to above-mentioned resulting medicament-carrying nano-fiber.Control revolving speed is 50rpm, and temperature is 37 ± 0.1 DEG C, dissolution
Medium selects the pH7.0 phosphate buffer solution of 900mL, and investigate has drug gradient distribution nanofiber with this condition
Vitro Drug controlled release properties.5mL is sampled on schedule, obtains dissolution fluid sample, and supplement same volume isothermal is fresh at once
Medium.After suitably being diluted to sample, in λmax At=264 nm, ultraviolet determination is carried out using ultraviolet-uisible spectrophotometer, is calculated
Medicine ibuprofen the amount of dissolution and accumulation dissolution percentage, are repeated 6 times.As a result as shown in fig. 6, it can be seen from the figure that due to medicine
The gradient distribution of object, although the drug release area of outer layer is big, drug diffusion is apart from short, and medicament contg is low, therefore fiber
The Initial burst effect of drug can be effectively eliminated.As drug release enters middle layer and internal layer, the area containing drug fiber is not
It is disconnected to reduce, while drug molecule extends from the distance that fibrous inside enters dissolution bulk solution, but due to the ladder of medicament contg
Degree increases, and effectively compensating for these leads to the ever-reduced factor of drug release, and drug is kept to release with constant rate uniform
It puts.
This zero-order drug controlled fashion obtained by drug gradient distribution is expected to overcome patient's initial stage blood concentration
Toxic side effect is caused by excessively high to strengthen drug safety, simultaneously because drug is able to maintain the slow equal of long period
Even release avoids blood concentration too low and loses therapeutic effect, avoids the frequent drug administration of patient, can increase the tolerance of patient
And convenience.
Embodiment 4: there is salicylic acid provided by drug gradient distribution nanofiber to delay controlled release properties
According to the spinning solution concocting method and implementing process condition of embodiment 1, preparing salicylic acid has the characteristics that gradient distribution
Three-decker nanofiber, according to embodiment 4 carry out vitro Drug dissolution experiment, to drug in sample at the nm of λ=302
Content be measured, to detect fiber to the controlled release properties of drug, the results showed that, apparent zero level control is presented in drug salicylic acid
Feature is released, is discharged 16 hours with the rate of homogeneous constant.
Claims (3)
1. a kind of medicament-carrying nano-fiber with drug gradient distribution, it is characterised in that: described including an inner sandwich layer
The periphery of inner sandwich layer is provided with middle layer, and the periphery of the middle layer is provided with extexine, the inner sandwich layer, middle layer and
Extexine coaxially extends, and drug is contained in the inner sandwich layer, middle layer and extexine, and the drug is dense from outside to inside
Degree successively increases in gradient；
A kind of preparation method of above-mentioned medicament-carrying nano-fiber with drug gradient distribution includes the following steps:
1) mother liquor is made into using spinnable polymer solution, and the mother liquor after preparing is divided into first part's mother liquor, second part
Mother liquor and Part III mother liquor；
2) medicine is added according to the increased sequence of concentration gradient in first part's mother liquor, second part mother liquor and Part III mother liquor
Object stirs evenly, and sequentially forms extexine working fluid, middle layer working fluid, inner sandwich layer working fluid, and corresponding loading is outer
Subsurface fluid syringe, middle layer fluid injector, in inner sandwich layer fluid injector, the one of the extexine fluid injector
End is connected with an appearance layer fluid syringe pump, one end of the middle layer fluid injector and an intermediate layer fluid injection
Pump connection, one end of the inner sandwich layer fluid injector is connected with an inner core layer fluid syringe pump, same using a three-level
Axis spinneret, the coaxial spinneret of the three-level include the coaxial capillary of internal layer, the coaxial capillary in middle layer, the coaxial capillary of outer layer
The inside of coaxial capillary in middle level is arranged in pipe, the coaxial capillary of the internal layer, and the coaxial capillary setting in the middle layer exists
The inside of the coaxial capillary of outer layer, the extexine fluid injector is connected with the coaxial capillary of the outer layer, described
Middle layer fluid injector is connected with the coaxial capillary in the middle layer, the inner sandwich layer fluid injector and the internal layer
Coaxial capillary connection, opens high pressure generator, controls three-layer fluid in the coaxial spinneret of three-level respectively by three syringe pumps
Injection rate, using the coaxial spinneret exit orifices of three-level as template, prepared with drug gradient point under the action of high-pressure electrostatic
The nanofiber of cloth feature, and plate is received by fiber and is received.
2. a kind of for printing the three-level coaxial electrically spun of the medicament-carrying nano-fiber with drug gradient distribution of claim 1
Device, it is characterised in that: including a coaxial spinneret of three-level, the coaxial spinneret of the three-level includes the coaxial capillary of internal layer
Pipe, the coaxial capillary in middle layer, the coaxial capillary of outer layer, the internal layer coaxial capillary setting coaxial capillary in middle level it is interior
The inside of the coaxial capillary of outer layer is arranged in portion, the coaxial capillary in the middle layer；It further include extexine fluid injector, centre
Layer fluid syringe, inner sandwich layer fluid injector, one end of the extexine fluid injector and an appearance layer fluid note
Pump connection is penetrated, one end of the middle layer fluid injector is connected with an intermediate layer fluid syringe pump, the inner sandwich layer
One end of fluid injector is connected with an inner core layer fluid syringe pump, the extexine fluid injector and the outer layer
Coaxial capillary connection, the middle layer fluid injector are connected with the coaxial capillary in the middle layer, the inner sandwich layer
Fluid injector is connected with the coaxial capillary of the internal layer；Further include a high pressure generator, the high pressure generator and
The coaxial spinneret connection of the three-level, the lower end of the outlet of the coaxial spinneret of the three-level is provided with fiber and receives plate.
3. three-level coaxial electrically spun device according to claim 2, it is characterised in that: the inner sandwich layer fluid injector and
Middle layer fluid injector pass through high resiliency silica gel hose in the coaxial spinneret of three-level the coaxial capillary of internal layer and middle layer
Coaxial capillary is connected.
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Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107272295B (en) * | 2017-07-14 | 2019-12-10 | 中国科学院广州能源研究所 | Flexible electrochromic fiber and method for preparing flexible electrochromic fiber by utilizing electrostatic spinning technology |
| CN107397974B (en) * | 2017-09-11 | 2020-08-04 | 安徽天耘医疗器械有限公司 | Wound plaster for treating chronic wound |
| CN111411403B (en) * | 2020-03-04 | 2021-03-05 | 扬州大学 | Electrostatic spinning preparation device of nanofiber filter screen and working method of electrostatic spinning preparation device |
| CN111910290B (en) * | 2020-07-27 | 2023-06-09 | 陕西科技大学 | Cobalt-nickel alloy/carbon composite electrocatalyst with gradient distribution and preparation method and application thereof |
| CN114908473B (en) * | 2022-03-28 | 2023-07-18 | 浙江理工大学 | Unidirectional moisture-conducting micro-nano fiber membrane with gradient pore structure and preparation method thereof |
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