CN114931638A - BFO-Zein/EC magnetic composite membrane material and preparation method and application thereof - Google Patents

BFO-Zein/EC magnetic composite membrane material and preparation method and application thereof Download PDF

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CN114931638A
CN114931638A CN202210566407.5A CN202210566407A CN114931638A CN 114931638 A CN114931638 A CN 114931638A CN 202210566407 A CN202210566407 A CN 202210566407A CN 114931638 A CN114931638 A CN 114931638A
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zein
bfo
magnetic composite
magnetic
preparation
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CN114931638B (en
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施文彦
董真佑
李海清
周任
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Ruinjin Hospital Affiliated to Shanghai Jiaotong University School of Medicine Co Ltd
University of Shanghai for Science and Technology
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    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K41/00—Medicinal preparations obtained by treating materials with wave energy or particle radiation ; Therapies using these preparations
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K47/00—Medicinal preparations characterised by the non-active ingredients used, e.g. carriers or inert additives; Targeting or modifying agents chemically bound to the active ingredient
    • A61K47/02—Inorganic compounds
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K47/00—Medicinal preparations characterised by the non-active ingredients used, e.g. carriers or inert additives; Targeting or modifying agents chemically bound to the active ingredient
    • A61K47/30—Macromolecular organic or inorganic compounds, e.g. inorganic polyphosphates
    • A61K47/36—Polysaccharides; Derivatives thereof, e.g. gums, starch, alginate, dextrin, hyaluronic acid, chitosan, inulin, agar or pectin
    • A61K47/38—Cellulose; Derivatives thereof
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K47/00—Medicinal preparations characterised by the non-active ingredients used, e.g. carriers or inert additives; Targeting or modifying agents chemically bound to the active ingredient
    • A61K47/30—Macromolecular organic or inorganic compounds, e.g. inorganic polyphosphates
    • A61K47/42—Proteins; Polypeptides; Degradation products thereof; Derivatives thereof, e.g. albumin, gelatin or zein

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  • Life Sciences & Earth Sciences (AREA)
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  • Animal Behavior & Ethology (AREA)
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Abstract

The invention belongs to the technical field of composite materials, and discloses a BFO-Zein/EC magnetic composite film material, and a preparation method and application thereof. The barium ferrite nano particles are modified by oleic acid, then are mixed with modified Zein fibers and stirred, are uniformly dispersed, are placed into a die to be die-cast into a film, and are magnetized, so that the BFO-Zein/EC magnetic film is obtained. The oleic acid modification improves the dispersion degree of barium ferrite nanoparticles and promotes the barium ferrite nanoparticles to be better combined with the modified zein fiber. Compared with the traditional exogenous magnetic field induced targeting material, the magnetic membrane material of the invention greatly simplifies the treatment steps and cost, has good biocompatibility, self-degradability and stable structure and magnetism, and can be applied to drug targeting in the medical field.

Description

BFO-Zein/EC magnetic composite membrane material and preparation method and application thereof
Technical Field
The invention relates to the technical field of composite materials, in particular to a BFO-Zein/EC magnetic composite film material and a preparation method and application thereof.
Background
The magnetic medicine target therapy is a therapeutic method which utilizes a magnetic field to lead the medicine with magnetic response to gather at a target position, improve the concentration of the medicine at the target position and reduce the toxicity and side effect of the medicine to normal tissues. At present, in-vivo magnetic drug targeting is induced by an in-vitro strong magnetic field mostly, but the in-vitro strong magnetic field induction has the problems of complicated treatment steps, complex required equipment, high treatment cost and the like. The spontaneous magnetic field induced targeting membrane material is expected to eliminate or improve the defects existing in the external strong magnetic field induced treatment. Therefore, development of a spontaneous magnetic field induced targeting membrane material and use thereof for magnetic drug targeting become a great need in the art.
Disclosure of Invention
In view of the above, the invention provides a BFO-Zein/EC magnetic composite membrane material, a preparation method and an application thereof, and solves the problem that the research of the current spontaneous magnetic field induced targeting membrane material is blank.
In order to achieve the purpose, the invention adopts the following technical scheme:
the invention provides a preparation method of a BFO-Zein/EC magnetic composite film material, which comprises the following steps:
s1: mixing ferric chloride, barium chloride, sodium hydroxide, oleic acid and water, separating precursor nano particles from the obtained mixed solution, and calcining to obtain BaFe 12 O 19 A nanoparticle;
s2: mixing zein, ethyl cellulose and an ethanol aqueous solution, and performing irradiation modification to obtain modified zein fibers;
s3: mixing BaFe 12 O 19 Mixing the nano particles and the modified Zein fiber, and magnetizing to obtain a BFO-Zein/EC magnetic composite membrane;
step S1 and step S2 have no sequential requirement.
Preferably, in step S1, the mixing manner of mixing the ferric chloride, the barium chloride, the sodium hydroxide, the oleic acid and the water is as follows: firstly, mixing ferric chloride, barium chloride and water, adding sodium hydroxide, stirring and mixing for 3-5 h, and then adding oleic acid.
Preferably, in step S1, the molar ratio of barium chloride to ferric chloride is 1: 9-14, wherein the volume concentration of oleic acid in the mixed solution is 5-50 mL/L, and the mass concentration of sodium hydroxide in the mixed solution is 20-200 g/L.
Preferably, in step S1, sodium hydroxide is added at 40-80 ℃.
Preferably, in the step S1, the calcination temperature is 700 to 1100 ℃, and the calcination time is 1 to 3 hours.
Preferably, in step S2, the mass ratio of the zein to the ethyl cellulose is 2 to 4: 1, the mass-volume ratio of the zein to the ethanol water solution is 1-3 g: 10mL, and the volume concentration of ethanol in the ethanol water solution is 60-80%.
Preferably, in the step S2, the irradiation modification is performed under a protective gas, the protective gas is nitrogen or hydrogen, and the irradiation dose is 50 to 100 KGy.
Preferably, in step S3, BaFe 12 O 19 The mass ratio of the nano particles to the modified zein fibers is 1-3: 1; before magnetizing, to BaFe 12 O 19 The mixture obtained by mixing the nano particles and the modified zein fiber is subjected to die-casting molding; the magnetizing magnetic field intensity is 0.5-5T.
The invention also provides a BFO-Zein/EC magnetic composite membrane material prepared by the preparation method of the BFO-Zein/EC magnetic composite membrane material.
The invention also provides application of the BFO-Zein/EC magnetic composite membrane material in preparing magnetic medicaments.
According to the technical scheme, compared with the prior art, the invention has the following beneficial effects:
BaFe of the invention 12 O 19 Has good magnetic property, stability and safety, can be uniformly dispersed in the film after being modified by oleic acid, and is tightly combinedSecret; zein (Zein) and Ethyl Cellulose (EC) are used as natural polymer materials, so that the natural polymer materials have good biocompatibility and film forming property, the load capacity of the natural polymer materials is greatly improved through crosslinking modification treatment, and the stability of the structure can be kept;
the method adopts the electron beam irradiation method to carry out crosslinking modification treatment on the material, has the advantages of environmental friendliness, continuous operation, batch treatment, low cost, small damage to the base material and the like, can achieve the sterilization effect, and greatly saves the steps;
the magnetic film material structure obtained by the method can keep stable magnetism for a long time, has obvious adsorption and aggregation effects on ferromagnetic particles, has positive significance on the development of endogenous magnetic targeting, and can be used for in vivo continuous drug targeting of chronic diseases.
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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 embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the provided drawings without creative efforts.
FIG. 1 is an XRD pattern of materials obtained in example 1 and comparative examples 1 to 2 of the present invention;
FIG. 2 is SEM pictures of materials obtained in example 1 and comparative examples 1-2 of the present invention, wherein (a) is a SEM picture of BFO NPs obtained in comparative example 2, (b) is a SEM picture of a BFO-Zein/EC magnetic film, and (c) is a SEM picture of a BFO-Zein magnetic film;
FIG. 3 is a VSM chart of materials obtained in example 1 and comparative examples 1 to 2 of the present invention.
Detailed Description
The invention provides a preparation method of a BFO-Zein/EC magnetic composite film material, which comprises the following steps:
s1: mixing ferric chloride, barium chloride, sodium hydroxide, oleic acid and water, separating precursor nano particles from the obtained mixed solution, and calcining to obtain BaFe 12 O 19 A nanoparticle;
s2: mixing zein, ethyl cellulose and an ethanol aqueous solution, and performing irradiation modification to obtain modified zein fibers;
s3: mixing BaFe 12 O 19 Mixing the nano particles and the modified Zein fiber, and magnetizing to obtain a BFO-Zein/EC magnetic composite membrane;
step S1 and step S2 have no sequential requirement.
In the invention, in step S1, the precursor nanoparticles are subjected to centrifugal drying treatment before being calcined; the rotation speed of the centrifugal drying is preferably 4000-12000 r/min, and further preferably 8000-11000 r/min; the centrifugal drying temperature is preferably 55-90 ℃, and further preferably 58-85 ℃; the time for centrifugal drying is preferably 10-14 h, and more preferably 11-13 h.
In the present invention, in step S1, the mixing manner of mixing the ferric chloride, the barium chloride, the sodium hydroxide, the oleic acid and the water is as follows: firstly, mixing ferric chloride, barium chloride and water, adding sodium hydroxide, stirring and mixing for 3-5 h, and then adding oleic acid;
the stirring and mixing time is preferably 3.5-4.5 h, and more preferably 220-250 min.
In the present invention, in the step S1, the ferric chloride is preferably ferric chloride containing crystal water, and more preferably FeCl 3 ·6H 2 O; the barium chloride is preferably barium chloride containing crystal water, and more preferably BaCl 2 ·2H 2 O。
In the present invention, in step S1, the molar ratio of barium chloride to ferric chloride is preferably 1: 9 to 14, and more preferably 1:10 to 13; the volume concentration of oleic acid in the mixed solution is preferably 5-50 mL/L, and more preferably 10-40 mL/L; the mass concentration of the sodium hydroxide in the mixed solution is preferably 20-200 g/L, and more preferably 50-150 g/L.
In the present invention, in the step S1, sodium hydroxide is preferably added at 40 to 80 ℃, and more preferably at 50 to 70 ℃.
In the invention, in the step S1, the calcination temperature is preferably 700-1100 ℃, and more preferably 800-1000 ℃; the calcination time is preferably 1 to 3 hours, and more preferably 1.5 to 2.5 hours.
In the present invention, in step S2, the mass ratio of the zein to the ethylcellulose is preferably 2 to 4: 1, more preferably 2.5-3.5: 1; the mass-volume ratio of the zein to the ethanol aqueous solution is preferably 1-3 g: 10mL, more preferably 1.5 to 2.5 g: 10 mL; the volume concentration of ethanol in the ethanol water solution is preferably 60-80%, and more preferably 65-75%.
In the present invention, in step S2, the irradiation modification is performed under a protective gas, and the protective gas is preferably nitrogen or hydrogen, and is more preferably nitrogen; the irradiation dose is preferably 50-100 KGy, and further preferably 60-80 KGy.
In the present invention, in the step S3, BaFe 12 O 19 The mass ratio of the nano particles to the modified zein fibers is preferably 1-3: 1, more preferably 1.5-2.5: 1; before magnetizing, to BaFe 12 O 19 The mixture obtained by mixing the nano particles and the modified zein fiber is subjected to die-casting forming; the magnetic field intensity of the magnetizing is preferably 0.5-5T, and more preferably 1-4T.
The invention also provides a BFO-Zein/EC magnetic composite membrane material prepared by the preparation method of the BFO-Zein/EC magnetic composite membrane material.
The invention also provides application of the BFO-Zein/EC magnetic composite membrane material in preparation of magnetic drugs.
The technical solutions provided by the present invention are described in detail below with reference to examples, but they should not be construed as limiting the scope of the present invention.
Example 1
16.2g FeCl 3 ·6H 2 O and 1.465g BaCl 2 ·2H 2 Dissolving O in 100mL of deionized water, adding 10g of sodium hydroxide at 60 ℃, continuously stirring for 4h, adding 2mL of oleic acid, and continuously stirring for 1h to obtain a precursor; centrifugally drying the obtained precursor at 5000r/min and 80 ℃ for 12h, and calcining at 900 ℃ for 2h to obtain BaFe 12 O 19 A nanoparticle;
dissolving 2g zein and 0.5g ethyl cellulose in 10mL 70% ethanol water solution, and filling with N 2 Bagging, carrying out irradiation modification, wherein the absorption dose is 80kGy, and then separating out the modified zein fiber;
2g of BaFe 12 O 19 Mixing and stirring the nano particles and 1g of modified Zein fiber for 30min, putting the mixture into a die to be die-cast into a membrane body with the thickness of 40mm multiplied by 1mm after the mixture is uniformly dispersed, and magnetizing the membrane body under the magnetic field strength of 2T to obtain the BFO-Zein/EC magnetic membrane.
Example 2
15g of FeCl 3 ·6H 2 O and 1.1g BaCl 2 ·2H 2 Dissolving O in 100mL of deionized water, adding 8g of sodium hydroxide at 70 ℃, continuously stirring for 4h, adding 1.5mL of oleic acid, and continuously stirring for 1h to obtain a precursor; centrifugally drying the obtained precursor at 9000r/min and 75 ℃ for 11h, and calcining at 1000 ℃ for 2.5h to obtain BaFe 12 O 19 A nanoparticle;
dissolving 2.5g zein and 1g ethyl cellulose in 10mL 80% ethanol water solution, and filling with N 2 Bagging, carrying out irradiation modification, and separating out the modified zein fiber, wherein the absorption dose is 60 kGy;
1g of BaFe 12 O 19 Mixing and stirring the nano particles and 1g of modified Zein fiber for 30min, putting the mixture into a die to be die-cast into a membrane body with the thickness of 40mm multiplied by 1mm after the mixture is uniformly dispersed, and magnetizing the membrane body under the magnetic field strength of 2T to obtain the BFO-Zein/EC magnetic membrane.
Comparative example 1
16.2g FeCl 3 ·6H 2 O and 1.465g BaCl 2 ·2H 2 Dissolving O in 100mL of deionized water, adding 10g of sodium hydroxide at 60 ℃, continuously stirring for 4h, adding 2mL of oleic acid, and continuously stirring for 1h to obtain a precursor; centrifugally drying the obtained precursor at 5000r/min and 80 ℃ for 12h, and calcining at 900 ℃ for 2h to obtain BaFe 12 O 19 A nanoparticle;
dissolving 2.5g zein in 10mL 70 vol%Filling N into ethanol water solution 2 Bagging, carrying out irradiation modification, wherein the absorption dose is 80kGy, and then separating out the modified zein fiber;
2g of BaFe 12 O 19 Stirring the nano particles and 1g of modified Zein fibers for 30min, uniformly dispersing, then putting into a die to be die-cast into a membrane body with the thickness of 40mm multiplied by 1mm, and magnetizing to obtain the BFO-Zein magnetic membrane.
Comparative example 2
16.2g FeCl 3 ·6H 2 O and 1.465g BaCl 2 ·2H 2 Dissolving O in 100mL of deionized water, adding 10g of sodium hydroxide at 60 ℃, continuously stirring for 4h, adding 2mL of oleic acid, and continuously stirring for 1h to obtain a precursor; centrifugally drying the obtained precursor at 5000r/min and 80 ℃ for 12h, and calcining at 900 ℃ for 2h to obtain BaFe 12 O 19 Nanoparticles, noted BFO NPs.
The materials obtained in example 1 and comparative examples 1 to 2 were tested, and the results are shown in FIGS. 1 to 3.
As can be seen from fig. 1, BFO NPs have distinct characteristic diffraction peaks corresponding to BaFe at 2 θ of 30.3, 32.2, 34.1, 37.1, 40.3, 42.4, 55.1, 56.3, 56.6, and 63.1 12 O 19 A nanoparticle; the diffraction peak of the BFO-Zein/EC magnetic film obtained by the invention is also very obvious in the spectrum, which shows that the magnetic particles have larger proportion in the magnetic film and have good magnetic performance.
As can be seen from FIG. 2, after the modification with oleic acid, the barium ferrite nanoparticles have uniform size distribution and good dispersibility, and the crystalline phase is a sheet hexagonal crystal with a size range of 50-200nm and is in the ranges of single domain critical size (460nm) and super paramagnetic critical size (14 nm); the surface of the magnetic film modified by cellulose forms ridges with the diameter of about 200nm, so that the material generates super-hydrophobicity, the water stability of the film is greatly improved, and meanwhile, barium ferrite is uniformly distributed on the magnetic film. The BFO-Zein/EC magnetic film obtained by the invention has more excellent stability and magnetic force performance compared with the BFO-Zein magnetic film and BFO NPs.
As can be seen from FIG. 3, the saturation magnetization of the BFO-Zein/EC magnetic film obtained by the invention is 44.75emu/g, the remanence is 24.84emu/g, and the coercive force is-4.8 k; the saturation magnetization of the BFO NPs is 65.19emu/g, the remanence is 33.32emu/g, and the coercive force is-4.8 k; the saturation magnetization of the BFO-Zein magnetic film is 43.32emu/g, the remanence is 23.41emu/g, and the coercive force is-4.8 k.
The BFO-Zein/EC magnetic film obtained by the invention not only has excellent magnetic force performance, but also has high stability, the magnetism can be kept stable for a long time, the BFO-Zein/EC magnetic film has obvious adsorption and aggregation effects on ferromagnetic particles, has positive significance on the development of endogenous magnetic targeting, and can be used for in vivo sustained drug targeting of chronic diseases.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.

Claims (10)

1. A preparation method of a BFO-Zein/EC magnetic composite film material is characterized by comprising the following steps:
s1: mixing ferric chloride, barium chloride, sodium hydroxide, oleic acid and water, separating precursor nano particles from the obtained mixed solution, and calcining to obtain BaFe 12 O 19 A nanoparticle;
s2: mixing zein, ethyl cellulose and an ethanol aqueous solution, and carrying out irradiation modification to obtain modified zein fibers;
s3: mixing BaFe 12 O 19 Mixing the nano particles and the modified Zein fiber, and magnetizing to obtain a BFO-Zein/EC magnetic composite membrane;
step S1 and step S2 have no sequential requirement.
2. The method for preparing the BFO-Zein/EC magnetic composite membrane material according to claim 1, wherein in step S1, the mixing manner of iron chloride, barium chloride, sodium hydroxide, oleic acid and water is: firstly, mixing ferric chloride, barium chloride and water, adding sodium hydroxide, stirring and mixing for 3-5 h, and then adding oleic acid.
3. The preparation method of the BFO-Zein/EC magnetic composite film material according to claim 2, wherein in step S1, the molar ratio of barium chloride to ferric chloride is 1: 9-14, wherein the volume concentration of oleic acid in the mixed solution is 5-50 mL/L, and the mass concentration of sodium hydroxide in the mixed solution is 20-200 g/L.
4. The preparation method of the BFO-Zein/EC magnetic composite film material as claimed in claim 3, wherein in step S1, sodium hydroxide is added at 40-80 ℃.
5. The preparation method of the BFO-Zein/EC magnetic composite film material as claimed in claim 1 or 2, wherein in the step S1, the calcination temperature is 700-1100 ℃, and the calcination time is 1-3 h.
6. The preparation method of the BFO-Zein/EC magnetic composite film material as claimed in claim 5, wherein in step S2, the mass ratio of Zein to ethyl cellulose is 2-4: 1, the mass-volume ratio of the zein to the ethanol water solution is 1-3 g: 10mL, and the volume concentration of ethanol in the ethanol water solution is 60-80%.
7. The preparation method of the BFO-Zein/EC magnetic composite film material as claimed in claim 6, wherein in the step S2, irradiation modification is performed under a protective gas, the protective gas is nitrogen or hydrogen, and the irradiation dose is 50-100 KGy.
8. The preparation method of the BFO-Zein/EC magnetic composite film material as claimed in any one of claims 1-4, wherein in the step S3, BaFe 12 O 19 The mass ratio of the nano particles to the modified zein fibers is 1-3: 1; before magnetizing, to BaFe 12 O 19 The mixture obtained by mixing the nano particles and the modified zein fiber is subjected to die-casting forming; the magnetizing magnetic field intensity is 0.5-5T.
9. The BFO-Zein/EC magnetic composite membrane material prepared by the method for preparing the BFO-Zein/EC magnetic composite membrane material as claimed in any one of claims 1-8.
10. The use of the BFO-Zein/EC magnetic composite membrane material of claim 9 in the preparation of magnetic pharmaceuticals.
CN202210566407.5A 2022-05-24 2022-05-24 BFO-Zein/EC magnetic composite film material and preparation method and application thereof Active CN114931638B (en)

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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1879065A (en) * 2003-09-12 2006-12-13 弗尔克斯破产财产公司 Magnetically targetable particles comprising magnetic components and biocompatible polymers for site-specific delivery of biologically active agents
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US20180085496A1 (en) * 2015-04-01 2018-03-29 Yale University Ferromagnetic particles bound to polymeric implants

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1879065A (en) * 2003-09-12 2006-12-13 弗尔克斯破产财产公司 Magnetically targetable particles comprising magnetic components and biocompatible polymers for site-specific delivery of biologically active agents
US20180085496A1 (en) * 2015-04-01 2018-03-29 Yale University Ferromagnetic particles bound to polymeric implants
CN106479196A (en) * 2016-11-04 2017-03-08 金福兴 A kind of antimicrobial packaging thin-film material and preparation method thereof

Non-Patent Citations (3)

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Title
MARIN, TIFFANY等: "Bioactive films of zein/magnetite magnetically stimuli-responsive for controlled drug release", 《JOURNAL OF MAGNETISM AND MAGNETIC MATERIALS》 *
卢杭诣: "水稳定zein基电纺纤维的制备及其药物释放行为研究", 《中国优秀硕士学位论文全文数据库工程科技Ⅰ辑》 *
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