CN106801261A - A kind of electro spinning nano fiber with medicine gradient distribution and preparation method thereof - Google Patents
A kind of electro spinning nano fiber with medicine gradient distribution and preparation method thereof Download PDFInfo
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- CN106801261A CN106801261A CN201710010815.1A CN201710010815A CN106801261A CN 106801261 A CN106801261 A CN 106801261A CN 201710010815 A CN201710010815 A CN 201710010815A CN 106801261 A CN106801261 A CN 106801261A
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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
Abstract
The invention provides a kind of medicament-carrying nano-fiber with medicine gradient distribution, including an inner sandwich layer, the periphery of described inner sandwich layer is provided with intermediate layer, the periphery in described intermediate layer is provided with extexine, described inner sandwich layer, intermediate layer and extexine coaxially extend, contain medicine in described inner sandwich layer, intermediate layer and extexine, concentration in gradient increases described medicine successively from outside to inside.Present invention also offers the preparation method of the above-mentioned nanofiber with medicine gradient distribution.Additionally provide the device for realizing the above method.Method of the present invention preparation process 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, and fiber surface is smooth.The medicine gradient distribution can be that the design of numerous sustained and controlled release medicine materials and preparation provide effective.
Description
Technical field
The invention belongs to materialogy field, it is related to a kind of structure-activity relationship establishing techniques of novel nano level material, specifically
For be a kind of electro spinning nano fiber with medicine gradient distribution and preparation method thereof.
Background technology
High-voltage electrostatic spinning technology（Electrospinning）It is a kind of nano-fabrication technique of (top-down) from top to bottom, by additional
Electric field force overcomes the jet that the surface tension of liquid and viscoelastic power of shower nozzle tip drop are formed, in electrostatic repulsion, Coulomb force and table
Under the tension force 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, nano-scale fiber is obtained after solvent volatilization or melt cooling in receiving terminal.The technical matters process is simple, manipulation side
Just, selection material ranges are extensive, controllability strong, be considered as the one kind for most possibly realizing continuous nano-fibre industrialized production
Method, preparing functional nano-fiber using the technology has good prospect.
Electric spinning polymer functional nano-fiber is general with fibre-forming polymer as base material, assigns and receiving by adding active component
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 component.These are only
Special performance includes that fibre diameter is small, fiber surface area is big, fiber is in three-dimensional netted loose structure, porosity be high, fiber has
The diameter of nanoscale scope but has length of macro-scope etc. simultaneously.In biomedicine field, typically medicine is added poly-
Polymer solution, forms solution altogether and, as spinning solution, by the rapid draing and shaping of common electro-spinning process, obtains medicaments uniformity
It is distributed in the medicament-carrying nano-fiber of whole nanofiber.Most medicament-carrying nano-fibers are all the distributions of such medicaments uniformity and tie
The single nanofiber of structure, obtains required medicine the characteristics of by the physicochemical property and nano fibrous membrane of polymeric substrate
Slow controlled release properties.Though have on a small quantity by the distribution of coaxial electrically spun and electrospinning regulating medicine arranged side by side in nanofiber, to obtain
The electrospinning core sheath nanofiber and Qiao Nasi nanofibers of medicine controlled releasing performance are needed, but on the nano junction of other structures feature
The preparation of structure, and these structures are applied in terms of the controlled release properties of medicine are provided and are seldom reported.
The content of the invention
For above-mentioned technical problem of the prior art, the invention provides a kind of electricity with medicine gradient distribution
Spinning nano fibre and preparation method thereof, described this electro spinning nano fiber and its preparation side with medicine gradient distribution
Method will solve the not good technical problem of medicine sustained and controlled release performance of the prior art.
The invention provides a kind of medicament-carrying nano-fiber with medicine gradient distribution, including an inner sandwich layer, institute
The periphery of the inner sandwich layer stated is provided with intermediate layer, and the periphery in described intermediate layer is provided with extexine, described inner sandwich layer, centre
Layer and extexine coaxially extend, and contain medicine in described inner sandwich layer, intermediate layer and extexine, and described medicine is by outward extremely
Interior concentration in gradient increases successively.
Present invention also offers a kind of above-mentioned medicament-carrying nano-fiber with medicine gradient distribution, including following step
Suddenly:
1) mother liquor is made into using spinnable polymer solution, and mother liquor after preparing is divided into Part I mother liquor, Part II
Mother liquor and Part III mother liquor；
2) medicine is added according to the increased order of concentration gradient in Part I mother liquor, Part II mother liquor and Part III mother liquor
Thing, stirs, and sequentially forms extexine working fluid, intermediate layer working fluid, inner sandwich layer working fluid, and correspondence loads outer
In subsurface fluid syringe, intermediate layer fluid injector, inner sandwich layer fluid injector, the one of described extexine fluid injector
Layer fluid injection in the middle of end and the connection of appearance layer fluid syringe pump, one end of described intermediate layer fluid injector and one
Pump is connected, one end of described inner sandwich layer fluid injector and an inner core layer fluid syringe pump connection, same using a three-level
Axle spinneret, the coaxial spinneret of described three-level includes the coaxial capillary of internal layer, the coaxial capillary in middle level, the coaxial capillary of outer layer
Pipe, the coaxial capillary of described internal layer is arranged on the inside of the coaxial capillary in middle level, and the coaxial capillary in described middle level is arranged on
The inside of the coaxial capillary of outer layer, the coaxial capillary connection of described extexine fluid injector and described outer layer is described
The coaxial capillary connection of intermediate layer fluid injector and described middle level, described inner sandwich layer fluid injector and described internal layer
Coaxial capillary connection, opens high pressure generator, and three-layer fluid in the coaxial spinneret of three-level is controlled respectively by three syringe pumps
Injection rate, in the presence of high-pressure electrostatic, with the coaxial spinneret exit orifices of three-level as template, prepare with medicine gradient point
The nanofiber of cloth feature, and flat board reception is received by fiber.
Present invention also offers the three-level coaxial electrically spun device for realizing the above method, including a coaxial spinneret of three-level,
The coaxial spinneret of described three-level includes the coaxial capillary of internal layer, the coaxial capillary in middle level, the coaxial capillary of outer layer, and described is interior
The coaxial capillary of layer is arranged on the inside of the coaxial capillary in middle level, and the coaxial capillary in described middle level is arranged on the coaxial capillary of outer layer
The inside of pipe；Also include extexine fluid injector, intermediate layer fluid injector, inner sandwich layer fluid injector, described appearance
One end of layer fluid syringe and the connection of appearance layer fluid syringe pump, one end and of described intermediate layer fluid injector
Individual middle layer fluid syringe pump connection, one end of described inner sandwich layer fluid injector and an inner core layer fluid syringe pump connect
Connect, the connection of described extexine fluid injector and described outer layer coaxial capillary, described intermediate layer fluid injector and
The coaxial capillary connection in described middle level, the coaxial capillary connection of described inner sandwich layer fluid injector and described internal layer；Also
Including a high pressure generator, the coaxial spinneret connection of described high pressure generator and described three-level, described three-level is coaxial
The lower end of the outlet of spinneret is provided with fiber and receives flat board.
Further, described inner sandwich layer and intermediate layer fluid injector are coaxial with three-level by high resiliency silica gel hose
Internal layer capillary in spinneret is connected with intermediate layer capillary.
Nanofiber of the invention by interior outer wrapping three-level core sheath structure feature；Fibrous inside medicine distribution gradient；
The Gradient Features refer to that, by intermediate layer to internal layer, the mode that drug delivery adds increases successively from outer layer；The structural fibers can be with
Effectively implement to prepare using three-level coaxial electrically spun technique single step, and the Zero order controlled releasing effect of medicine can be provided.
The present invention is compared with prior art, and its technological progress is significant.The present invention is that one kind passes through medicine in the fibre
Gradient distribution obtain needed for medicine Zero order controlled releasing performance electro spinning nano fiber.Method of the present invention preparation process is simple, it is 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,
Fiber surface is smooth.The medicine gradient distribution can provide effectively real for the design of numerous sustained and controlled release medicine materials and preparation
Applying method.
Brief description of the drawings
Fig. 1 is the Taylor cone observation figures that the coaxial technique of three-level that the present invention is used prepares nanofiber.
Fig. 2 three-level coaxial electrically spun technology implementation schematic diagrams.1- high pressure generators；The outer layer fluid syringe pumps of 2-；In 3-
Between fluid syringe pump；4- internal layer fluid syringe pumps；The coaxial spinneret of 5- three-levels；6- fiber receiver sheets；7- high resiliency silica gel hoses；
8- outer layer fluid injectors；9- central fluid syringes；10- internal layer fluid injectors.
Fig. 3 is the scanning electron microscope diagram with medicine gradient distribution nanofiber of the invention.
Fig. 4 is the transmission electron microscope figure with medicine gradient distribution nanofiber of the invention.
Fig. 5 is structural representation of the present invention with medicine gradient distribution nanofiber.
The medicine Zero order controlled releasing figure that Fig. 6 is provided by nanofiber of the invention.
Specific embodiment
Below in conjunction with drawings and Examples, the present invention is described in detail.These embodiments be only used for explain the present invention and
It is not intended to the limitation present invention.All uses and same or analogous method of the invention, or the equivalent modifications made, all should fall into this
Invention protection domain.
Embodiment 1：The implementation of three-level coaxial electrically spun technique
36 grams of vinyl acetate celluloses are put into 300 grams by acetone and N,N-dimethylformamide in mass ratio 3:1 composition it is mixed
In bonding solvent, the mother liquor with favorable spinning quality is made into.Above-mentioned mother liquor is divided into three parts, medicine is separately added into wherein
1 gram, 3 grams and 5 grams of thing chlorphenamine maleate, by being stirred into transparent solution altogether, serves as internal layer, intermediate layer
With the working fluid of outer layer.Above-mentioned three kinds of working fluids are respectively charged into inner sandwich layer, intermediate layer and the appearance of three-level coaxial electrically spun
In the syringe 10,9,8 of layer working fluid, in each layer fluid of connection to the coaxial spinneret 5 of three-level, high-pressure spinning head and height are connected
Pressure electrostatic generator 1.Implement three-level coaxial high pressure electrostatic spinning process according to following technological parameter：Internal layer/centre/outer layer
Fluid flow is 0.8/0.8/0.8 mL/h, and receiver board is 20 cm, the kV of voltage 14 with a distance from spinning nozzle.Environment temperature is (21
± 3) DEG C, ambient humidity is 61 ± 5 %.In the above operating condition, bust shot in situ, electrospinning mistake are carried out to electro-spinning process
Journey is as shown in figure 1, the three-layer fluid from the coaxial spinneret of three-level out is collectively forming a compound Taylor cone, the top of cone
A straight jet is sent, straight jet is followed by the unstable region of high frequency stretching.Prepared nanofiber passes through one
The aluminium foil parcel cardboard of ground connection is collected.
Realize the three-level coaxial electrically spun device of the above method（Such as Fig. 2）, including a coaxial spinneret 5 of three-level, it is described
The coaxial spinneret 5 of three-level is made up of internal layer capillary, intermediate layer capillary and the coaxial capillary of outer layer；Also include an inner sandwich layer
Fluid injector 10, intermediate layer fluid injector 9 and an extexine fluid injector 8；Described inner sandwich layer fluid injector
10 one end and an inner core layer fluid syringe pump 4 are connected, and one end of intermediate layer fluid injector 9 and a middle layer fluid are noted
Penetrate pump 3 to connect, one end of outer layer fluid injector 8 and an outer layer fluid syringe pump 2 are connected, described inner core layer fluid injection
The other end of device 10 and the connection of described internal layer coaxial capillary, the other end of intermediate layer fluid injector 9 and described
The coaxial capillary connection in middle level, the coaxial capillary connection of outer layer described in the other end of extexine fluid injector 8, also includes
One high pressure generator 1, the described coaxial spinneret 5 of high pressure generator 1 and described three-level is connected, and described three-level is coaxially spun
The lower end of first 5 outlet of silk is provided with the fiber reception flat board 6 that the hardboard wrapped up with aluminium foil is made.
Further, described inner sandwich layer and intermediate 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 intermediate layer capillary.
Embodiment 2：Phenetic analysis with medicine gradient distribution nanofiber pattern Yu structure
Using field emission scanning electron microscope（FESEM）Observed after surface metal spraying is carried out to fiber prepared by embodiment 1, as a result such as Fig. 3
It is shown.Prepared fiber is presented good linear condition, do not have that bead structure, fiber surface be smooth, fiber accumulations are equal
It is even.A diameter of 640 ± 130 nm, than more uniform, concentration is compared in diameter distribution for distribution.
Using high resolution transmission electron microscopy（TEM）Prepared fibrous inner structure is observed, as a result such as Fig. 4 institutes
Show, nanofiber it is interior/in/outer three-decker is clear, wherein outer layer because medicament contg is few and thickness of thin, so present compared with
Low gray scale, internal layer medicament contg is big, and thickness is big, therefore larger gray scale is presented.
As shown in figure 5, a kind of described medicament-carrying nano-fiber with medicine gradient distribution is inner sandwich layer 11, centre
The three-level core sheath structure of the interior outer wrapping that layer 22 and extexine 33 are constituted, wherein, from extexine 33 by intermediate layer 33 to inner core
Layer 22, the content of drug molecule 44 increases distribution in gradient.
Embodiment 3：With the slow controlled release properties of brufen that medicine gradient distribution nanofiber is provided
By D drug release determinations the second method slurry processes of 2015 editions annex of Chinese Pharmacopoeia Ⅹ, using RCZ-8A intelligence dissolution experiment instruments to upper
The medicament-carrying nano-fiber for stating gained carries out In Vitro Dissolution experiment.Rotating speed is controlled for 50rpm, temperature is 37 ± 0.1 DEG C, dissolution medium
From the pH7.0 PBSs of 900mL, the medicine with medicine gradient distribution nanofiber is investigated with this understanding
The outer controlled release properties of object.5mL is sampled on schedule, dissolution fluid sample is obtained, and supplements same volume isothermal fresh medium at once.
After to the appropriate dilution of sample, in λmax At=264 nm, ultraviolet determination is carried out using ultraviolet-uisible spectrophotometer, calculate medicine
Brufen stripping quantity and accumulation dissolution percentage, are repeated 6 times.Result is as shown in fig. 6, it can be seen that due to medicine
Gradient is distributed, although the medicine release area of outer layer is big, apart from short, medicament contg is low, therefore fiber can for drug diffusion
Effectively eliminate the Initial burst effect of medicine.As insoluble drug release enters intermediate layer and internal layer, the area containing drug fiber constantly subtracts
It is small, while the distance that drug molecule enters dissolution bulk solution from fibrous inside extends, but because the gradient of medicament contg increases
Greatly, effectively compensate for these causes the ever-reduced factor of insoluble drug release, keeps medicine to be discharged with constant rate uniform.
This zero-order drug controlled fashion for being distributed and being obtained by medicine gradient, is expected to overcome patient's initial stage blood concentration
Toxic and side effect is so as to strengthen drug safety caused by too high, simultaneously because medicine can keep the slow equal of long period
Even release, it is to avoid blood concentration is too low and loses therapeutic effect, it is to avoid the frequent drug administration of patient, by increasing capacitance it is possible to increase the tolerance of patient
And convenience.
Embodiment 4：With the slow controlled release properties of salicylic acid that medicine gradient distribution nanofiber is provided
According to the spinning solution concocting method and implementing process condition of embodiment 1, preparing salicylic acid has the three of gradient characteristic distributions
Rotating fields nanofiber, vitro Drug dissolution experiment is carried out according to embodiment 4, at the nm of λ=302 to sample in medicine contain
Amount is measured, and with detection fibers to the controlled release properties of medicine, as a result shows, it is special that medicine salicylic acid is presented obvious Zero order controlled releasing
Levy, discharged 16 hours with the speed of homogeneous constant.
Claims (4)
1. a kind of medicament-carrying nano-fiber with medicine gradient distribution, it is characterised in that:It is described including an inner sandwich layer
The periphery of inner sandwich layer is provided with intermediate layer, and the periphery in described intermediate layer is provided with extexine, described inner sandwich layer, intermediate layer and
Extexine coaxially extends, and medicine is contained in described inner sandwich layer, intermediate layer and extexine, and described medicine is dense from outside to inside
Degree increases successively in gradient.
2. a kind of medicament-carrying nano-fiber with medicine gradient distribution described in claim 1, it is characterised in that including such as
Lower step:
1）Mother liquor is made into using spinnable polymer solution, and mother liquor after preparing is divided into Part I mother liquor, Part II
Mother liquor and Part III mother liquor；
2）In Part I mother liquor, Part II mother liquor and Part III mother liquor medicine is added according to the increased order of concentration gradient
Thing, stirs, and sequentially forms extexine working fluid, intermediate layer working fluid, inner sandwich layer working fluid, and correspondence loads outer
In subsurface fluid syringe, intermediate layer fluid injector, inner sandwich layer fluid injector, the one of described extexine fluid injector
Layer fluid injection in the middle of end and the connection of appearance layer fluid syringe pump, one end of described intermediate layer fluid injector and one
Pump is connected, one end of described inner sandwich layer fluid injector and an inner core layer fluid syringe pump connection, same using a three-level
Axle spinneret, the coaxial spinneret of described three-level includes the coaxial capillary of internal layer, the coaxial capillary in middle level, the coaxial capillary of outer layer
Pipe, the coaxial capillary of described internal layer is arranged on the inside of the coaxial capillary in middle level, and the coaxial capillary in described middle level is arranged on
The inside of the coaxial capillary of outer layer, the coaxial capillary connection of described extexine fluid injector and described outer layer is described
The coaxial capillary connection of intermediate layer fluid injector and described middle level, described inner sandwich layer fluid injector and described internal layer
Coaxial capillary connection, opens high pressure generator, and three-layer fluid in the coaxial spinneret of three-level is controlled respectively by three syringe pumps
Injection rate, in the presence of high-pressure electrostatic, with the coaxial spinneret exit orifices of three-level as template, prepare with medicine gradient point
The nanofiber of cloth feature, and flat board reception is received by fiber.
3. the three-level coaxial electrically spun device of claim 2 methods described is realized, it is characterised in that：Including a coaxial spinning of three-level
Head, the coaxial spinneret of described three-level includes the coaxial capillary of internal layer, the coaxial capillary in middle level, the coaxial capillary of outer layer, described
The coaxial capillary of internal layer be arranged on the inside of the coaxial capillary in middle level, it is coaxial that the coaxial capillary in described middle level is arranged on outer layer
The inside of capillary；Also include extexine fluid injector, intermediate layer fluid injector, inner sandwich layer fluid injector, it is described
One end of extexine fluid injector and the connection of appearance layer fluid syringe pump, one end of described intermediate layer fluid injector
With one in the middle of the connection of layer fluid syringe pump, one end of described inner sandwich layer fluid injector and an inner core layer fluid syringe pump
Connection, the coaxial capillary connection of described extexine fluid injector and described outer layer, described intermediate layer fluid injector
With the described coaxial capillary connection in middle level, the coaxial capillary connection of described inner sandwich layer fluid injector and described internal layer；
Also include a high pressure generator, the coaxial spinneret connection of described high pressure generator and described three-level, described three-level is same
The lower end of the outlet of axle spinneret is provided with fiber and receives flat board.
4. three-level coaxial electrically spun device according to claim 3, it is characterised in that：Described inner sandwich layer and middle layer fluid
Syringe is connected by the internal layer capillary and intermediate layer capillary in the coaxial spinneret of high resiliency silica gel hose and three-level.
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| CN111411403A (en) * | 2020-03-04 | 2020-07-14 | 扬州大学 | Electrostatic spinning preparation device of nanofiber filter screen and working method of electrostatic spinning preparation device |
| CN111910290A (en) * | 2020-07-27 | 2020-11-10 | 陕西科技大学 | Cobalt-nickel alloy/carbon composite electrocatalyst with gradient distribution and preparation method and application thereof |
| CN114908473A (en) * | 2022-03-28 | 2022-08-16 | 浙江理工大学 | One-way moisture-conducting micro-nanofiber membrane with gradient pore structure and preparation method thereof |
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| CN114908473A (en) * | 2022-03-28 | 2022-08-16 | 浙江理工大学 | One-way moisture-conducting micro-nanofiber membrane with gradient pore structure and preparation method thereof |
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| CN106801261B (en) | 2019-05-24 |
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