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CN113564768A - Preparation method of antibacterial electrostatic spinning nano yarn convenient to collect - Google Patents

Preparation method of antibacterial electrostatic spinning nano yarn convenient to collect Download PDF

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Publication number
CN113564768A
CN113564768A CN202110823344.2A CN202110823344A CN113564768A CN 113564768 A CN113564768 A CN 113564768A CN 202110823344 A CN202110823344 A CN 202110823344A CN 113564768 A CN113564768 A CN 113564768A
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CN
China
Prior art keywords
electrostatic spinning
nano
antibacterial
yarn
spinning
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN202110823344.2A
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Chinese (zh)
Inventor
杨军政
王彬
秦大江
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Fifth Affiliated Hospital of Guangzhou Medical University
Original Assignee
Fifth Affiliated Hospital of Guangzhou Medical University
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Fifth Affiliated Hospital of Guangzhou Medical University filed Critical Fifth Affiliated Hospital of Guangzhou Medical University
Priority to CN202110823344.2A priority Critical patent/CN113564768A/en
Publication of CN113564768A publication Critical patent/CN113564768A/en
Pending legal-status Critical Current

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    • DTEXTILES; PAPER
    • D02YARNS; MECHANICAL FINISHING OF YARNS OR ROPES; WARPING OR BEAMING
    • D02GCRIMPING OR CURLING FIBRES, FILAMENTS, THREADS, OR YARNS; YARNS OR THREADS
    • D02G3/00Yarns or threads, e.g. fancy yarns; Processes or apparatus for the production thereof, not otherwise provided for
    • D02G3/44Yarns or threads characterised by the purpose for which they are designed
    • D02G3/449Yarns or threads with antibacterial properties
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B82NANOTECHNOLOGY
    • B82YSPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00Manufacture or treatment of nanostructures
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01DMECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
    • D01D5/00Formation of filaments, threads, or the like
    • D01D5/0007Electro-spinning
    • D01D5/0015Electro-spinning characterised by the initial state of the material
    • D01D5/003Electro-spinning characterised by the initial state of the material the material being a polymer solution or dispersion
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01DMECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
    • D01D5/00Formation of filaments, threads, or the like
    • D01D5/0007Electro-spinning
    • D01D5/0061Electro-spinning characterised by the electro-spinning apparatus
    • D01D5/0076Electro-spinning characterised by the electro-spinning apparatus characterised by the collecting device, e.g. drum, wheel, endless belt, plate or grid
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01FCHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F1/00General methods for the manufacture of artificial filaments or the like
    • D01F1/02Addition of substances to the spinning solution or to the melt
    • D01F1/10Other agents for modifying properties
    • D01F1/103Agents inhibiting growth of microorganisms
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01FCHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F6/00Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
    • D01F6/88Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds
    • D01F6/92Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds of polyesters
    • DTEXTILES; PAPER
    • D02YARNS; MECHANICAL FINISHING OF YARNS OR ROPES; WARPING OR BEAMING
    • D02GCRIMPING OR CURLING FIBRES, FILAMENTS, THREADS, OR YARNS; YARNS OR THREADS
    • D02G3/00Yarns or threads, e.g. fancy yarns; Processes or apparatus for the production thereof, not otherwise provided for
    • D02G3/02Yarns or threads characterised by the material or by the materials from which they are made
    • DTEXTILES; PAPER
    • D02YARNS; MECHANICAL FINISHING OF YARNS OR ROPES; WARPING OR BEAMING
    • D02GCRIMPING OR CURLING FIBRES, FILAMENTS, THREADS, OR YARNS; YARNS OR THREADS
    • D02G3/00Yarns or threads, e.g. fancy yarns; Processes or apparatus for the production thereof, not otherwise provided for
    • D02G3/22Yarns or threads characterised by constructional features, e.g. blending, filament/fibre
    • DTEXTILES; PAPER
    • D10INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
    • D10BINDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
    • D10B2401/00Physical properties
    • D10B2401/13Physical properties anti-allergenic or anti-bacterial

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  • Engineering & Computer Science (AREA)
  • Textile Engineering (AREA)
  • Chemical & Material Sciences (AREA)
  • Mechanical Engineering (AREA)
  • General Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Manufacturing & Machinery (AREA)
  • Nanotechnology (AREA)
  • Physics & Mathematics (AREA)
  • Condensed Matter Physics & Semiconductors (AREA)
  • General Physics & Mathematics (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Dispersion Chemistry (AREA)
  • Spinning Methods And Devices For Manufacturing Artificial Fibers (AREA)
  • Agricultural Chemicals And Associated Chemicals (AREA)

Abstract

The invention discloses a preparation method of antibacterial electrostatic spinning nano yarn, which is convenient to collect and comprises the following steps: preparing PLA or PLGA electrostatic spinning solution containing norfloxacin or ciprofloxacin lactate, placing the PLA or PLGA electrostatic spinning solution or electrostatic spraying solution containing norfloxacin or ciprofloxacin lactate on an electrostatic spinning machine to manufacture nano-fibers, wherein a receiving device adopts a tray filled with purified water, the nano-fibers naturally float on the surface of the tray filled with purified water to form a layer of electrostatic spinning film, taking a relatively thin copper wire, rolling up the electrostatic spinning film in parallel to form nano-yarn, and 3, placing the manufactured nano-yarn in a ventilation cabinet or a test bench for natural drying. The technical scheme of the invention improves the mechanical strength, porosity and drug release effect of the nano-fiber, wraps the antibacterial drug, has good antibacterial effect, and can ensure the integrity of the electrostatic spinning membrane because the receiving medium is water and the obtained electrostatic spinning membrane is easy to collect.

Description

Preparation method of antibacterial electrostatic spinning nano yarn convenient to collect
Technical Field
The invention relates to the technical field of electrostatic spinning nano-fibers, in particular to a preparation method of antibacterial electrostatic spinning nano-yarn convenient to collect.
Background
The electrostatic spinning nanofiber has good application value in the fields of tissue regeneration and medicine due to the large pore structure and excellent drug loading performance. The electrostatic spinning nanofiber membrane obtained by the existing electrostatic spinning technology has poor mechanical performance, and the pore structure or drug-loading property is often limited due to the single structure; and the receiving device is mainly a metal receiving device such as tin foil paper, so that the electrostatic spinning film is difficult to peel off from the metal receiving device such as tin foil paper, and the electrostatic spinning film is easy to damage in the peeling process, so that the original appearance structure of the electrostatic spinning film is damaged.
Accordingly, the prior art is deficient and needs improvement.
Disclosure of Invention
The invention mainly aims to provide a preparation method of an electrostatic spinning nano yarn which is convenient to collect and antibacterial, and aims to facilitate the collection of an electrostatic spinning membrane and further improve the pore structure, the mechanical property and the drug-loaded drug release effect of the electrostatic spinning nanofiber membrane.
In order to achieve the purpose, the preparation method of the electrostatic spinning nano yarn which is convenient to collect and antibacterial comprises the following steps:
s1: preparing spinning solution
Dissolving a spinning solute in an organic solvent, and adding an antibacterial drug, wherein the mass-to-volume ratio of the spinning solute to the organic solvent is 10-12%, the mass-to-volume ratio of the antibacterial drug to the organic solvent is 0.3-0.7%, the spinning solute comprises one or a combination of two of PLGA or PLA, the antibacterial drug comprises one or a combination of two of norfloxacin or ciprofloxacin lactate, and the organic solvent comprises one or a combination of at least two of chloroform, acetone and N, N-dimethylformamide;
s2: carrying out electrostatic spinning on the spinning solution
And (4) putting the spinning solution prepared in the step (S1) into an electrostatic spinning machine for electrostatic spinning, wherein the electrostatic spinning machine comprises the following electric spraying conditions: the voltage is 20-30kV, the receiving distance is 7cm, the propelling speed of the injector is 0.5mL/h, the ambient temperature is 20-30 ℃, the humidity is 60-70%, and the receiving device of the electrostatic spinning membrane is provided with a bearing liquid for bearing the electrostatic spinning membrane;
s3: preparation of electrospun Nanoproins
And when the electrostatic spinning film reaches a certain thickness, taking out the receiving device, and parallelly rolling up the electrostatic spinning film on the surface of the bearing liquid through a copper wire to form the electrostatic spinning nano yarn.
Preferably, the spinning solute is provided as PLA.
Preferably, the antibacterial drug is configured as norfloxacin.
Preferably, the organic solvent comprises chloroform, acetone and N, N-dimethylformamide, and the volume ratio of the chloroform to the acetone to the N, N-dimethylformamide is 2: 1: 3.
preferably, the receiving means is provided as a tray.
Preferably, the carrier liquid is provided as purified water.
Preferably, the method further comprises the step of placing the formed electrostatic spinning nano yarn in a fume hood or a test bed for natural airing.
Compared with the prior art, the invention has the beneficial effects that:
1. the method has simple flow and convenient operation and implementation;
2. the tray filled with purified water is used as a receiving device, so that the obtained electrostatic spinning film is easy to collect and can be further processed without damaging the original appearance structure;
3. the microsphere interface or the nanofiber membrane is made of the green, environment-friendly and pollution-free PLA material, and has good biocompatibility;
4. the electrostatic spinning nano yarn prepared by the method further improves the mechanical property, the porosity and the drug-loading property on the basis of electrostatic spinning nano fibers;
5. the electrostatic spinning nano yarn prepared by the method is coated with norfloxacin or ciprofloxacin lactate with antibacterial effect, and has good practical value in the field of biomedicine.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the structures shown in the drawings without creative efforts.
FIG. 1 is a schematic illustration of an electrospinning process of the present invention;
FIG. 2 is a schematic diagram of an electrospinning nano-yarn manufacturing process of the present invention;
FIG. 3 is a schematic representation of an electrospun membrane of the invention wrapped with norfloxacin;
the implementation, functional features and advantages of the objects of the present invention will be further explained with reference to the accompanying drawings.
Detailed Description
The preparation method of the antibacterial electrospun nano yarn convenient to collect provided by the embodiment comprises the following steps of:
s1: preparing spinning solution
Dissolving a spinning solute in an organic solvent, and adding an antibacterial drug, wherein the mass-to-volume ratio of the spinning solute to the organic solvent is 10-12%, the mass-to-volume ratio of the antibacterial drug to the organic solvent is 0.3-0.7%, the spinning solute comprises one or a combination of two of PLGA or PLA, the antibacterial drug comprises one or a combination of two of norfloxacin or ciprofloxacin lactate, and the organic solvent comprises one or a combination of at least two of chloroform, acetone and N, N-dimethylformamide;
s2: carrying out electrostatic spinning on the spinning solution
And (4) putting the spinning solution prepared in the step (S1) into an electrostatic spinning machine for electrostatic spinning, wherein the electrostatic spinning machine comprises the following electric spraying conditions: the voltage is 20-30kV, the receiving distance is 7cm, the propelling speed of the injector is 0.5mL/h, the ambient temperature is 20-30 ℃, the humidity is 60-70%, and the receiving device of the electrostatic spinning membrane is provided with a bearing liquid for bearing the electrostatic spinning membrane;
s3: preparation of electrospun Nanoproins
And when the electrostatic spinning film reaches a certain thickness, taking out the receiving device, and parallelly rolling up the electrostatic spinning film on the surface of the bearing liquid through a copper wire to form the electrostatic spinning nano yarn.
Further, the spinning solute is PLA, the antibacterial agent is norfloxacin, the organic solvent comprises chloroform, acetone and N, N-dimethylformamide, and the volume ratio of the chloroform to the acetone to the N, N-dimethylformamide is 2: 1: 3.
further, the receiving device is arranged as a tray, and the carrier liquid is pure water.
It should be noted that, in this embodiment, the nano yarn with various specifications of different diameters or lengths can be obtained according to actual production requirements, the mechanical strength, the porosity and the drug release effect of the nano yarn are improved, norfloxacin or ciprofloxacin lactate is wrapped, so that the nano yarn has a good antibacterial effect, and the obtained electrostatic spinning film is easily collected because the receiving medium is water, so that the integrity of the electrostatic spinning film can be ensured, and the nano yarn has a good application prospect.
Further, the formed electrostatic spinning nano yarn is placed in a fume hood or a test bed to be naturally dried.
The present application is illustrated below by way of specific examples:
taking 10mL of electrostatic spinning solution system as an example, 5mL of N, N-dimethylformamide, 3.4mL of chloroform and 1.7mL of acetone are accurately measured by a measuring cylinder; 1.2g of PLA material and 0.04g of norfloxacin are weighed by an electronic balance, then the weighed PLA and norfloxacin are poured into a mixed chloroform/acetone/N, N dimethylformamide solution, and stirred for 1.5h by shaking until the PLA is completely dissolved;
and (3) putting the prepared spinning solution into an electrostatic spinning machine for electrostatic spinning, wherein the electrostatic spinning machine comprises the following electric spraying conditions: the voltage is 20-30kV, the receiving distance is 7cm, the advancing speed of the injector is 0.5mL/h, the ambient temperature is 25 ℃, the humidity is 65%, and the receiving device is a tray filled with purified water;
after the electrostatic spinning reaches a certain thickness, taking out the tray, and replacing the tray filled with the purified water to continue receiving the electrostatic spinning; and placing the taken tray containing the electrostatic spinning film on a platform, taking a thin copper wire, and rolling the electrostatic spinning film in parallel to form the nano yarn, wherein the thickness and the length of the nano yarn can be adjusted according to requirements. Then placing the mixture in a ventilated place for natural airing.
Further, the nano yarn prepared in the above example was subjected to an antibacterial test, the procedure was as follows:
1. preparing and sterilizing an agar culture medium;
2. preparation of bacterial suspension: in a clean bench, Staphylococcus aureus and Escherichia coli colonies were scraped with a sterile cotton swab to a sterile NaCl-peptone solution at pH 7.0, 6X 108comparing cfu/mL turbidimetric tubes, performing gradient dilution after the concentration is reached, and obtaining the final bacterial liquid concentration of 6 x 105cfu/mL, followed by 6 x 10 dip with sterile cotton swab5Evenly smearing cfu/mL solution on a trypticase soy peptone agar culture medium culture dish;
3. pasting and placing the bacteriostatic sample: and (3) shearing a sample piece with the diameter and the area of 5mm from the prepared electrostatic spinning membrane, slightly pressing the sample piece into a culture dish coated with bacteria, covering the culture dish, and placing the culture dish in an incubator for culturing for 16-18 h.
4. And (3) judging the bacteriostatic action: the antibacterial ring is larger than 7mm, and has antibacterial effect.
Specifically, the bacteriostatic effect of the nano yarn prepared in this example is shown in the following table:
escherichia coli Staphylococcus aureus
Sample 1 21.33mm 17.31mm
Sample 2 22.15mm 19.41mm
Sample 3 19.44mm 19.23mm
The above description is only a preferred embodiment of the present invention, and not intended to limit the scope of the present invention, and all modifications of equivalent structures and equivalent processes, which are made by using the contents of the present specification and the accompanying drawings, or directly or indirectly applied to other related technical fields, are included in the scope of the present invention.

Claims (7)

1. A preparation method of antibacterial electrospun nano yarn convenient to collect is characterized by comprising the following steps:
s1: preparing spinning solution
Dissolving a spinning solute in an organic solvent, and adding an antibacterial drug, wherein the mass-to-volume ratio of the spinning solute to the organic solvent is 10-12%, the mass-to-volume ratio of the antibacterial drug to the organic solvent is 0.3-0.7%, the spinning solute comprises one or a combination of two of PLGA or PLA, the antibacterial drug comprises one or a combination of two of norfloxacin or ciprofloxacin lactate, and the organic solvent comprises one or a combination of at least two of chloroform, acetone and N, N-dimethylformamide;
s2: carrying out electrostatic spinning on the spinning solution
And (4) putting the spinning solution prepared in the step (S1) into an electrostatic spinning machine for electrostatic spinning, wherein the electrostatic spinning machine comprises the following electric spraying conditions: the voltage is 20-30kV, the receiving distance is 7cm, the propelling speed of the injector is 0.5mL/h, the ambient temperature is 20-30 ℃, the humidity is 60-70%, and the receiving device of the electrostatic spinning membrane is provided with a bearing liquid for bearing the electrostatic spinning membrane;
s3: preparation of electrospun Nanoproins
And when the electrostatic spinning film reaches a certain thickness, taking out the receiving device, and parallelly rolling up the electrostatic spinning film on the surface of the bearing liquid through a copper wire to form the electrostatic spinning nano yarn.
2. The method for preparing easy-to-collect and antibacterial electrospun nano yarn according to claim 1 wherein the spinning solute is PLA.
3. The method of preparing a collectable, antimicrobial electrospun nano-yarn of claim 1 wherein the antimicrobial drug is norfloxacin.
4. The method of preparing easy-to-collect and antibacterial electrospun nano yarn according to claim 1 wherein the organic solvent comprises chloroform, acetone and N, N dimethylformamide and the volume ratio between chloroform, acetone and N, N dimethylformamide is 2: 1: 3.
5. the method of claim 1, wherein the receiving device is configured as a tray.
6. The method of preparing easy-to-collect and anti-microbial electrospun nano-yarns according to claim 5 wherein the carrier liquid is provided as purified water.
7. The method for preparing easy-to-collect and antibacterial electrospun nano-yarn according to any one of claims 1 to 6, further comprising placing the formed electrospun nano-yarn in a fume hood or a test bed for natural airing.
CN202110823344.2A 2021-07-20 2021-07-20 Preparation method of antibacterial electrostatic spinning nano yarn convenient to collect Pending CN113564768A (en)

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Application Number Priority Date Filing Date Title
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Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103100116A (en) * 2012-12-31 2013-05-15 范存义 Tissue adhesion prevention material, medicine-carrying material and preparation method thereof
KR20160129784A (en) * 2015-04-30 2016-11-09 고려대학교 산학협력단 Manufacturing method for high dispersion fiber aggregate having expanded inter-fiber space and manufacturing apparatus for the same
CN106149203A (en) * 2016-07-22 2016-11-23 东华大学 A kind of medicament-carrying nano-fiber membrane and application thereof
KR101857204B1 (en) * 2017-06-23 2018-05-11 포항공과대학교 산학협력단 Water electrospinning device and fabricating method of fiber membrane using the same
CN108866649A (en) * 2018-08-21 2018-11-23 杭州卫达生物材料科技有限公司 A kind of collection device and method for electrostatic spinning
CN109942843A (en) * 2019-02-12 2019-06-28 新乡医学院三全学院 A kind of PLGA superhydrophobic surface with antibacterial effect and preparation method thereof
CN112981558A (en) * 2021-02-23 2021-06-18 苏州大学 Electrostatic spinning device and preparation method of ZnO-PLGA-PCL antibacterial nanofiber membrane

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103100116A (en) * 2012-12-31 2013-05-15 范存义 Tissue adhesion prevention material, medicine-carrying material and preparation method thereof
KR20160129784A (en) * 2015-04-30 2016-11-09 고려대학교 산학협력단 Manufacturing method for high dispersion fiber aggregate having expanded inter-fiber space and manufacturing apparatus for the same
CN106149203A (en) * 2016-07-22 2016-11-23 东华大学 A kind of medicament-carrying nano-fiber membrane and application thereof
KR101857204B1 (en) * 2017-06-23 2018-05-11 포항공과대학교 산학협력단 Water electrospinning device and fabricating method of fiber membrane using the same
CN108866649A (en) * 2018-08-21 2018-11-23 杭州卫达生物材料科技有限公司 A kind of collection device and method for electrostatic spinning
CN109942843A (en) * 2019-02-12 2019-06-28 新乡医学院三全学院 A kind of PLGA superhydrophobic surface with antibacterial effect and preparation method thereof
CN112981558A (en) * 2021-02-23 2021-06-18 苏州大学 Electrostatic spinning device and preparation method of ZnO-PLGA-PCL antibacterial nanofiber membrane

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Application publication date: 20211029