CN104947229A - Method for preparing medicine-carrying nanofibers of core-shell structure by virtue of Pickering emulsion electrospinning - Google Patents
Method for preparing medicine-carrying nanofibers of core-shell structure by virtue of Pickering emulsion electrospinning Download PDFInfo
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Abstract
The invention relates to a method for preparing medicine-carrying nanofibers of a core-shell structure by virtue of Pickering emulsion electrospinning. The method comprises the following steps: 1) the preparation of a Pickering emulsion; 2) the electrospinning of the Pickering emulsion, namely sucking the Pickering emulsion obtained in the step 1) into a 10ml injector, connecting an injection pump with a receiving device, and preparing the nanofibers of the Pickering emulsion by virtue of electrospinning under the conditions of a DC voltage within the range of 15-25kV, an injection rate within the range of 0.1ml/h to 1.0ml/h and an interval between the receiving plate and the needle head of the injector within the range of 15cm to 20cm. Compared with the prior art, the method has the advantages that no any small molecular surfactant having biotoxicity needs to be added to the prepared Pickering emulsion as an emulsifier and the specific functions of nanoparticles are introduced to the Pickering emulsion, and therefore, the Pickering emulsion has specific advantages in application in the fields such as medicine release and tissue engineering.
Description
Technical field
The present invention relates to the preparation method of the medicament-carrying nano-fiber with nucleocapsid structure, particularly relate to a kind of method being prepared nucleocapsid structure medicament-carrying nano-fiber by Pickering emulsion electrostatic spinning.
Background technology
Utilizing the high polymer nanometer fiber that electrostatic spinning is obtained, is a kind of good medicine carrying material.On the one hand, according to the common recognition of pathology educational circles, the specific area of medicine and pharmaceutical carrier is larger, and the decomposition rate of drug particles is faster.The diameter dimension of nanofiber, at Nano grade, makes nanofiber have huge surface area, utilizes it as medicine carrying material, and the medicine that some can be made originally to be difficult to be absorbed by the body can decompose release lentamente, plays result for the treatment of.On the other hand, utilize degradable or absorbable polymer material as medicine carrying matrix, can by the privileged site of medicine implant into body in a specified pattern, along with the release of medicine, medicine carrying material by the hydrolysis natural degradation of carbochain, can not damage to human body.
In recent years, researcher utilizes electrospinning to prepare to have the nanofiber pharmaceutical carrier of nucleocapsid structure.The medicine loaded, at stratum nucleare, is conducive to the activity keeping medicine; The existence of shell can hinder the violent release of medicine further, and by change its composition and character carry out Drug controlled release behavior.Utilize electrospinning to prepare nuclear shell structure nano fiber pharmaceutical carrier, usually have coaxial electrically spun and emulsion electrospinning two kinds of modes.Such as, publication number is disclose a kind of preparation method utilizing coaxial electrically spun technology to prepare medical dressing nucleocapsid structure superfine fiber carrier material in the patent of CN103611182A.Compared with coaxial electrically spun, the operation of emulsion electrospinning is more simple, a step can obtain the medicament-carrying nano-fiber with nucleocapsid structure.And for example publication number is disclose a kind of method that emulsion Electrospinning Method prepares Biodegradable polyester fiber in the patent of CN103572508A.But, conventional emulsion needs to add Small molecular surfactant usually, such as, take charge of class 80 etc., keep stability, and these surfactants often have bio-toxicity, because which limit the application of the nano-fiber material prepared by conventional emulsion electrospinning at biomedicine field.Take nano particle as the deficiency that the Pickering emulsion electrospinning of stabilizing agent then can overcome conventional emulsion electrospinning.According to the own characteristic of these nano particles, the performance of polymer nanofiber in optics, mechanics, electricity or magnetics etc. can also be given.The nano particle that can be used for stable Pickering emulsion comprises nano ferriferrous oxide, CNT, graphene oxide, halloysite nanotubes, Nano diamond, nano silicon, Nano Silver, nano-titanium etc.Such as publication number is disclose a kind of method that Pickering emulsion electrospinning prepares linear structure fiber in the patent of CN103757728A, and the emulsifying agent wherein used just relates to nano silicon, and the nanofiber of preparation is linear structure.The present invention relates to use and there is amphipathic modified Nano particle prepare Pickering emulsion as emulsifying agent, then successfully prepared the medicament-carrying nano-fiber with nucleocapsid structure by the method for electrostatic spinning, the medicament-carrying nano-fiber of this structure has a good application prospect in the field such as drug controlled release and organizational project.
Summary of the invention
Technical problem to be solved by this invention is for above-mentioned prior art and proposes a kind of method being prepared nucleocapsid structure medicament-carrying nano-fiber by Pickering emulsion electrostatic spinning.
The present invention solves the problems of the technologies described above adopted technical scheme: a kind of method being prepared nucleocapsid structure medicament-carrying nano-fiber by Pickering emulsion electrostatic spinning, includes following steps:
1) preparation of Pickering emulsion: be first distributed in 10g ~ 20g two end number mixing organic solvent obtain modified Nano particle dispersion by having the amphipathic ultrasonic 30min ~ 60min of modified Nano particle emulsifying agent, then 1g ~ 2g polymer to be joined in 10g ~ 20g two end number mixing organic solvent and fully to dissolve under magnetic agitation condition, then being joined under the condition of room temperature high-speed stirred as oil phase by this polymer solution above-mentionedly has in amphipathic modified Nano particle dispersion, finally contain the aqueous solution 1.5ml ~ 2.5ml of 40mg ~ 60mg medicine toward above-mentioned mixed solution and dripping with the speed of 10ml/h ~ 20ml/h, obtain mixing homogeneous Pickering emulsion,
2) electrostatic spinning of Pickering emulsion: the Pickering emulsion of step (1) gained is sucked in 10ml syringe, connects syringe pump and receiving system.Be 15 ~ 25kV at DC voltage, injection rate is 0.1ml/h ~ 1.0ml/h, and under dash receiver is the condition of 15cm ~ 20cm to syringe needle spacing, electrospinning prepares the nanofiber of Pickering emulsion.
By such scheme, the described preparation method with amphipathic modified Nano particle emulsifying agent is: be distributed in deionized water by ultrasonic for 100mg ~ 200mg nano particle 30min ~ 60min, obtain the dispersion liquid that mass fraction is 10% ~ 20%, then under agitation, inject 5ml ~ 15ml oleic acid with the speed of 5 ~ 15ml/h, prepare and there is amphipathic modified Nano particle emulsifying agent.
By such scheme, described nano particle is: any one in nano ferriferrous oxide, CNT, graphene oxide, halloysite nanotubes, Nano diamond, nano silicon, Nano Silver and nano-titanium.
By such scheme, described polymer is: PLA, PGA, poly (glycolide-lactide), poly-epsilon-caprolactone, polyglycolic acid etc.; Described medicine comprises: any one in vancomycin, Ciprofloxacin Hydrochloride, Amoxicillin and quadracycline.
By such scheme, described binary mixed solvent is any two kinds in oxolane, chloroform, acetone and DMF, and its mass ratio is 1:9 ~ 9:1.
Compared with the prior art comparatively, advantage of the present invention is as follows:
(1) the present invention substitutes conventional emulsifier prepare Pickering emulsion to have amphipathic modified Nano particle;
(2) the present invention has amphipathic modified Nano particle content and profit phase volume ratio regulates and controls Pickering emulsion intercalation method by adjustment;
(3) the Pickering emulsion one step electrospinning of preparation is directly become the medicament-carrying nano-fiber with nucleocapsid structure by the method for electrostatic spinning by the present invention;
(4) the present invention has the volume ratio of amphipathic modified Nano particle content and profit phase by adjustment thus reaches the object of regulation and control nanofiber Chinese traditional medicine Co ntrolled release ability;
(5) the Pickering emulsion prepared of the present invention is without the need to adding any Small molecular surfactant with bio-toxicity as emulsifying agent, and introduce the specific function of nano particle self, in the middle of the application in the field such as insoluble drug release and organizational project, there is specific advantage.
Accompanying drawing explanation
The transmission electron microscope picture with the PLA Pickering emulsion electrospinning medicament-carrying nano-fiber of nucleocapsid structure that Fig. 1 obtains for embodiment 1;
The drug release patterns figure to take charge of PLA emulsion electrospinning medicament-carrying nano-fiber that class 80 is emulsifying agent and PLA Pickering emulsion electrospinning medicament-carrying nano-fiber with nucleocapsid structure that Fig. 2 obtains for embodiment 2;
The 1. pure polylactic acid electrospinning that Fig. 3 obtains for embodiment 3,2. to take charge of PLA emulsion electrospinning medicament-carrying nano-fiber that class 80 prepares for emulsifying agent with 3. PLA Pickering emulsion electrospinning medicament-carrying nano-fiber to the antibacterial effect comparison diagram of staphylococcus aureus.
Detailed description of the invention
Below in conjunction with embodiment, the present invention will be further described in detail.
Embodiment 1
(1) there is the preparation of amphipathic improved ferroferric oxide nano particle emulsifying agent: be distributed in deionized water by ultrasonic for 100mg tri-iron tetroxide 30min and obtain the dispersion liquid that mass fraction is 10%, under agitation, inject 5ml oleic acid with the speed of 5ml/h, obtained have amphipathic oleic acid modified Nano particle emulsifying agent;
(2) preparation of Pickering emulsion: first the amphipathic improved ferroferric oxide nano particle that has that step (1) is obtained is distributed to 1g N as the ultrasonic 30min of emulsifying agent, in the mixed solvent of dinethylformamide and 9g chloroform, then 1.0g PLA is joined 1g N, in the mixed organic solvents of dinethylformamide and 9g chloroform, fully dissolve under magnetic agitation condition, then being joined under the condition of room temperature high-speed stirred as oil phase by this solution above-mentionedly has in amphipathic improved ferroferric oxide nanoparticle dispersion liquid, finally contain the aqueous solution of 40mg Ciprofloxacin Hydrochloride toward above-mentioned mixed solution and dripping 1.5ml with the speed of 10ml/h, just can obtain mixing homogeneous Pickering emulsion,
(3) electrostatic spinning of Pickering emulsion: Pickering emulsion step (2) prepared sucks in 10ml syringe, connects syringe pump and receiving system.Be 15kV at DC voltage, injection rate is 0.1ml/h, and under dash receiver is the condition of 15cm to syringe needle spacing, electrospinning prepares the nanofiber of Pickering emulsion;
(4) preparation 1. pure polylactic acid electrospinning fibre, 2. with take charge of the PLA emulsion that class 80 prepares for emulsifying agent electro spinning nano fiber and 3. PLA Pickering emulsion medicament-carrying nano-fiber etc. the sample of quality, sample is placed on the solid medium being coated with staphylococcus aureus bacterium liquid, 37 DEG C of constant temperature culture 24h, contrast the antibacterial ability of three by the size comparing three sample antibacterial circle diameters.
Be illustrated in figure 1 the transmission electron microscope picture of the Pickering emulsion electrospinning drug-loading fibre of the PLA of preparation.Its structure is the fiber with inside and outside two-layer nucleocapsid structure as can be seen from Figure, and its stratum nucleare and shell mark with arrow all in the drawings.
Embodiment 2
(1) there is the preparation of amphipathic modified manometer silicon dioxide particle emulsifying agent: be distributed in deionized water by ultrasonic for 150mg nano-silicon dioxide particle 60min and obtain the dispersion liquid that mass fraction is 15%, under agitation, inject 10ml oleic acid with the speed of 10ml/h, obtained have amphipathic oleic acid modified manometer silicon dioxide particle emulsifying agent;
(2) preparation of Pickering emulsion: first the amphipathic modified manometer silicon dioxide particle that has that step (1) is obtained is distributed in the mixed solvent of 10g oxolane and 10g chloroform as the ultrasonic 60min of emulsifying agent, then 1.5g poly-epsilon-caprolactone is joined in the mixed organic solvents of 10g oxolane and 10g chloroform and fully dissolve under magnetic agitation condition, then being joined under the condition of room temperature high-speed stirred as oil phase by this solution above-mentionedly has in amphipathic modified manometer silicon dioxide particle dispersion, finally contain the aqueous solution of 50mg Amoxicillin toward above-mentioned mixed solution and dripping 2.0ml with the speed of 15ml/h, just can obtain mixing homogeneous Pickering emulsion,
(3) electrostatic spinning of Pickering emulsion: Pickering emulsion step (2) prepared sucks in 10ml syringe, connects syringe pump and receiving system.Be 20kV at DC voltage, injection rate is 0.5ml/h, and under dash receiver is the condition of 20cm to syringe needle spacing, electrospinning prepares the nanofiber of Pickering emulsion;
(4) preparation 1. pure poly-epsilon-caprolactone electrospinning, 2. with take charge of the poly-epsilon-caprolactone emulsion that class 80 prepares for emulsifying agent electro spinning nano fiber and 3. poly-epsilon-caprolactone Pickering emulsion medicament-carrying nano-fiber etc. the sample of quality, sample is placed on the solid medium being coated with staphylococcus aureus bacterium liquid, 37 DEG C of constant temperature culture 24h, contrast the antibacterial ability of three by the size comparing three sample antibacterial circle diameters.
Be illustrated in figure 2 Pickering emulsion electrospinning fibre and be drug release patterns figure in the phosphate buffer of the 0.1mol/L of 7.4 at pH to take charge of emulsion electrospinning fibre that class 80 is emulsifying agent.As can be seen from the figure, the time that Pickering emulsion electrospinning fibre reaches when release balances reaches 500 hours, is greater than the emulsion electrospun fiber membrane that the class of department 80 is emulsifying agent and reaches release balance required time (400 hours).Further, during release balance, the cumulative release percentage (58%) of Pickering emulsion electrospinning drug-loading fibre is also greater than the cumulative release percentage (51%) of the emulsion electrospinning drug-loading fibre that the class of department 80 is emulsifying agent.This illustrates that the sustained drug release effect of Pickering emulsion electrospinning drug-loading fibre is better than the emulsion electrospinning drug-loading fibre that the class of department 80 is emulsifying agent.
Embodiment 3
(1) there is the preparation of amphipathic improved ferroferric oxide nano particle emulsifying agent: be distributed in deionized water by ultrasonic for 200mg nano ferriferrous oxide 60min and obtain the dispersion liquid that mass fraction is 20%, under agitation, inject 15ml oleic acid with the speed of 15ml/h, prepare oleic acid modified Nano particle emulsifying agent;
(2) preparation of Pickering emulsion: first the amphipathic improved ferroferric oxide nano particle that has that step (1) is obtained is distributed to 18g N as the ultrasonic 60min of emulsifying agent, in the mixed solvent of dinethylformamide and 2g acetone, then 2.0g PLA is joined 18g N, in the mixed organic solvents of dinethylformamide and 2g acetone, fully dissolve under magnetic agitation condition, then being joined under the condition of room temperature high-speed stirred as oil phase by this solution above-mentionedly has in amphipathic improved ferroferric oxide nanoparticle dispersion liquid, finally contain the aqueous solution of 60mg vancomycin toward above-mentioned mixed solution and dripping 2.5ml with the speed of 20ml/h, just can obtain mixing homogeneous Pickering emulsion,
(3) electrostatic spinning of Pickering emulsion: the Pickering emulsion that step (2) is prepared is poured in 10ml syringe, connects syringe pump and receiving system.Be 25kV at DC voltage, injection rate is 1.0ml/h, and under dash receiver is the condition of 25cm to syringe needle spacing, electrospinning prepares the nanofiber of Pickering emulsion;
(4) preparation 1. pure polylactic acid electrospinning, 2. with take charge of the PLA emulsion that class 80 prepares for emulsifying agent electro spinning nano fiber and 3. PLA Pickering emulsion medicament-carrying nano-fiber etc. the sample of quality, sample is placed on the solid medium being coated with staphylococcus aureus bacterium liquid, 37 DEG C of constant temperature culture 24h, contrast the antibacterial ability of three by the size comparing three sample antibacterial circle diameters.
Antibacterial experiment as shown in Figure 3 compares the anti-microbial property of above-mentioned three kinds of fibers, and pure polylactic acid electrospinning does not almost occur inhibition zone, shows almost do not have antibiotic property.And to take charge of the Pickering emulsion medicament-carrying nano-fiber of PLA emulsion electrospinning medicament-carrying nano-fiber that class 80 prepares for emulsifying agent and PLA, respectively the inhibition zone that diameter is 10mm and 22mm is demonstrated to staphylococcus aureus.This illustrates, compared to take charge of the PLA emulsion electrospinning medicament-carrying nano-fiber that class 80 prepares for emulsifying agent, the PLA Pickering emulsion electrospinning medicament-carrying nano-fiber membrane containing improved ferroferric oxide nano particle with nucleocapsid structure has stronger antibacterial ability.
Claims (5)
1. prepared a method for nucleocapsid structure medicament-carrying nano-fiber by Pickering emulsion electrostatic spinning, include following steps:
1) preparation of Pickering emulsion: be first distributed in 10g ~ 20g two end number mixing organic solvent obtain modified Nano particle dispersion by having the amphipathic ultrasonic 30min ~ 60min of modified Nano particle emulsifying agent, then 1g ~ 2g polymer to be joined in 10g ~ 20g two end number mixing organic solvent and fully to dissolve under magnetic agitation condition, then being joined under the condition of room temperature high-speed stirred as oil phase by this polymer solution above-mentionedly has in amphipathic modified Nano particle dispersion, finally contain the aqueous solution 1.5ml ~ 2.5ml of 40mg ~ 60mg medicine toward above-mentioned mixed solution and dripping with the speed of 10ml/h ~ 20ml/h, obtain mixing homogeneous Pickering emulsion,
2) electrostatic spinning of Pickering emulsion: the Pickering emulsion of step (1) gained is sucked in 10ml syringe, connects syringe pump and receiving system.Be 15 ~ 25kV at DC voltage, injection rate is 0.1ml/h ~ 1.0ml/h, and under dash receiver is the condition of 15cm ~ 20cm to syringe needle spacing, electrospinning prepares the nanofiber of Pickering emulsion.
2. method according to claim 1, it is characterized in that, the described preparation method with amphipathic modified Nano particle emulsifying agent is: be distributed in deionized water by ultrasonic for 100mg ~ 200mg nano particle 30min ~ 60min, obtain the dispersion liquid that mass fraction is 10% ~ 20%, then under agitation, inject 5ml ~ 15ml oleic acid with the speed of 5 ~ 15ml/h, prepare and there is amphipathic modified Nano particle emulsifying agent.
3. method according to claim 2, it is characterized in that, described nano particle is: any one in nano ferriferrous oxide, CNT, graphene oxide, halloysite nanotubes, Nano diamond, nano silicon, Nano Silver and nano-titanium.
4. method according to claim 1, is characterized in that, described polymer is: PLA, PGA, poly (glycolide-lactide), poly-epsilon-caprolactone, polyglycolic acid etc.; Described medicine comprises: any one in vancomycin, Ciprofloxacin Hydrochloride, Amoxicillin and quadracycline.
5. method according to claim 1, is characterized in that, described binary mixed solvent is any two kinds in oxolane, chloroform, acetone and DMF, and its mass ratio is 1:9 ~ 9:1.
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CN105603553B (en) * | 2015-11-03 | 2018-01-26 | 江苏擎宇化工科技有限公司 | HNTs preparation method and the method for preparing the method for high polymer/HNTs mixed liquors using HNTs and high polymer nano fiber being prepared using mixed liquor |
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CN107115570B (en) * | 2017-03-30 | 2020-06-19 | 华南理工大学 | Nano composite biological scaffold with multi-stage controllable through hole structure and preparation method and application thereof |
CN108479780A (en) * | 2018-05-08 | 2018-09-04 | 宁波工程学院 | A kind of preparation method of optomagnetic response halloysite nanotubes hollow microsphere |
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CN113773520B (en) * | 2021-07-27 | 2022-12-16 | 海南大学 | Preparation method of in-situ degradable alginic acid base drug-loaded nanofiber membrane |
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CN113578190B (en) * | 2021-09-02 | 2022-07-19 | 四川冠山科技有限公司 | Switch Pickering emulsion with stable low-concentration particles and preparation method thereof |
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