CN114931638B - BFO-Zein/EC magnetic composite film material and preparation method and application thereof - Google Patents

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

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CN114931638B
CN114931638B CN202210566407.5A CN202210566407A CN114931638B CN 114931638 B CN114931638 B CN 114931638B CN 202210566407 A CN202210566407 A CN 202210566407A CN 114931638 B CN114931638 B CN 114931638B
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zein
bfo
magnetic composite
magnetic
composite film
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CN114931638A (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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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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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 subjected to oleic acid modification, then are mixed and stirred with modified Zein fibers, are uniformly dispersed, are put into a die for die casting to form a film, and are subjected to magnetizing treatment to obtain the BFO-Zein/EC magnetic film. The oleic acid modification improves the dispersion degree of the barium ferrite nano-particles and promotes better combination with the modified zein fiber. Compared with the traditional exogenous magnetic field induced targeting material, the magnetic film material greatly simplifies the treatment steps and cost, has good biocompatibility, self-degradability, stable structure and magnetism, and can be applied to drug targeting in the medical field.

Description

BFO-Zein/EC magnetic composite film 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 drug targeting treatment is a treatment method which utilizes a magnetic field to gather a drug with magnetic response at a target site, improves the concentration of the drug at the target site, and reduces the toxicity and side effects of the drug to normal tissues. At present, in-vivo magnetic drug targeting mostly adopts in-vitro strong magnetic field induction, but in-vitro strong magnetic field induction has the problems of complicated treatment steps, complex required equipment, high treatment cost and the like. The self-magnetic field induced targeting membrane material is expected to eliminate or improve the defects existing in-vitro strong magnetic field induced treatment. Therefore, the development of spontaneous magnetic field induced targeting membrane materials and their use in magnetic drug targeting is highly desirable 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 application thereof, and solves the problem that the research of the existing spontaneous magnetic field induced targeting membrane material is blank.
In order to achieve the above 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, ethylcellulose and ethanol aqueous solution, and carrying out irradiation modification to obtain modified zein fibers;
s3: baFe is added to 12 O 19 Mixing the nano particles with modified Zein fibers, and magnetizing to obtain a BFO-Zein/EC magnetic composite film;
step S1 and step S2 are not sequentially required.
Preferably, in the 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 the 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 the step S1, sodium hydroxide is added at 40 to 80 ℃.
Preferably, in the step S1, the calcination temperature is 700 to 1100 ℃ and the calcination time is 1 to 3 hours.
Preferably, in the step S2, the mass ratio of zein to ethylcellulose is 2 to 4:1, the mass volume ratio of zein to ethanol aqueous solution is 1-3 g:10mL, 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, wherein the protective gas is nitrogen or hydrogen, and the irradiation dose is 50-100 KGy.
Preferably, in the step S3, baFe 12 O 19 The mass ratio of the nano particles to the modified zein fibers is 1-3: 1, a step of; before magnetizing, baFe 12 O 19 The mixture obtained by mixing the nano particles and the modified zein fibers is subjected to die casting molding; the intensity of the magnetized magnetic field is 0.5-5T.
The invention also provides the BFO-Zein/EC magnetic composite film material prepared by the preparation method of the BFO-Zein/EC magnetic composite film material.
The invention also provides application of the BFO-Zein/EC magnetic composite film material in preparing magnetic medicines.
Compared with the prior art, the invention has the following beneficial effects:
BaFe according to the invention 12 O 19 The modified oleic acid-containing magnetic material has good magnetic performance, stability and safety, can be uniformly dispersed in a film after being modified by oleic acid, and is tightly combined; the Zein (Zein) and the Ethylcellulose (EC) are taken as natural polymer materials, have good biocompatibility and film forming property, and greatly improve the load capacity through crosslinking modification treatment, and can keep the stability of the structure;
the invention adopts the electron beam irradiation method to carry out crosslinking modification treatment on the material, and the method has the advantages of environmental protection, continuous operation, batch treatment, low cost, little damage to the base material and the like, can also achieve the sterilization effect, and greatly saves the steps;
the magnetic film material structure obtained by the method can keep magnetism stable for a long time, has obvious adsorption and aggregation effects on ferromagnetic particles, has positive significance on development of endogenous magnetic targeting, and can be used for in vivo continuous drug targeting of chronic diseases.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings that are required to be used in the embodiments or the description of the prior art will be briefly described below, and it is obvious that the drawings in the following description are only embodiments of the present invention, and that other drawings can be obtained according to the provided drawings without inventive effort for a person skilled in the art.
FIG. 1 is an XRD pattern of the materials obtained in example 1 and comparative examples 1 to 2 of the present invention;
FIG. 2 is an SEM image of the materials obtained in example 1 and comparative examples 1-2 of the present invention, wherein (a) is an SEM image of BFO NPs obtained in comparative example 2, (b) is an SEM image of BFO-Zein/EC magnetic film, and (c) is an SEM image of BFO-Zein magnetic film;
FIG. 3 is a VSM chart of the 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, ethylcellulose and ethanol aqueous solution, and carrying out irradiation modification to obtain modified zein fibers;
s3: baFe is added to 12 O 19 Mixing the nano particles with modified Zein fibers, and magnetizing to obtain a BFO-Zein/EC magnetic composite film;
step S1 and step S2 are not sequentially required.
In the present invention, in the step S1, centrifugal drying treatment is performed before calcination of the precursor nanoparticles; the rotation speed of centrifugal drying is preferably 4000-12000 r/min, more preferably 8000-11000 r/min; the temperature of centrifugal drying is preferably 55 to 90 ℃, and more preferably 58 to 85 ℃; the centrifugal drying time is preferably 10 to 14 hours, more preferably 11 to 13 hours.
In the present invention, in the 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 hours, and then adding oleic acid;
the stirring and mixing time is preferably 3.5 to 4.5 hours, more preferably 220 to 250 minutes.
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 the step S1, the molar ratio of barium chloride to ferric chloride is preferably 1:9 to 14, more preferably 1:10 to 13; the volume concentration of oleic acid in the mixed solution is preferably 5-50 mL/L, more preferably 10-40 mL/L; the mass concentration of sodium hydroxide in the mixed solution is preferably 20 to 200g/L, more preferably 50 to 150g/L.
In the present invention, in the step S1, sodium hydroxide is preferably added at 40 to 80 ℃, and more preferably sodium hydroxide is added at 50 to 70 ℃.
In the present invention, in the step S1, the temperature of calcination is preferably 700 to 1100 ℃, and more preferably 800 to 1000 ℃; the calcination time is preferably 1 to 3 hours, more preferably 1.5 to 2.5 hours.
In the present invention, in the step S2, the mass ratio of zein to ethylcellulose is preferably 2 to 4:1, more preferably 2.5 to 3.5:1; the mass volume ratio of zein to ethanol water solution is preferably 1-3 g:10mL, more preferably 1.5 to 2.5g:10mL; the volume concentration of ethanol in the aqueous ethanol solution is preferably 60 to 80%, more preferably 65 to 75%.
In the present invention, in the step S2, the irradiation modification is performed under a protective gas, preferably nitrogen or hydrogen, and more preferably nitrogen; the irradiation dose is preferably 50 to 100KGy, more preferably 60 to 80KGy.
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 to 2.5:1;before magnetizing, baFe 12 O 19 The mixture obtained by mixing the nano particles and the modified zein fibers is subjected to die casting molding; the magnetizing field strength is preferably 0.5 to 5T, more preferably 1 to 4T.
The invention also provides the BFO-Zein/EC magnetic composite film material prepared by the preparation method of the BFO-Zein/EC magnetic composite film material.
The invention also provides application of the BFO-Zein/EC magnetic composite film material in preparing magnetic medicines.
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 O is dissolved in 100mL of deionized water, 10g of sodium hydroxide is added at 60 ℃ for continuous stirring for 4 hours, 2mL of oleic acid is added for continuous stirring for 1 hour, and a precursor is obtained; centrifuging and drying the obtained precursor at 5000r/min and 80 ℃ for 12 hours, and calcining at 900 ℃ for 2 hours to obtain BaFe 12 O 19 A nanoparticle;
dissolving 2g zein and 0.5g ethyl cellulose in 10mL 70% ethanol water solution by volume and filling N 2 Bagging, carrying out irradiation modification, and separating out the modified zein fiber after the absorbed dose is 80 kGy;
2g of BaFe 12 O 19 The nano particles and 1g of modified Zein fiber are mixed and stirred for 30min, the mixture is put into a die after being uniformly dispersed, a film body with the thickness of 40mm multiplied by 1mm is formed by die casting, and magnetizing treatment is carried out under the strength of a 2T magnetic field, so that the BFO-Zein/EC magnetic film is obtained.
Example 2
15g FeCl 3 ·6H 2 O and 1.1g BaCl 2 ·2H 2 O is dissolved in 100mL of deionized water, 8g of sodium hydroxide is added at 70 ℃ for continuous stirring for 4 hours, 1.5mL of oleic acid is added for continuous stirring for 1 hour, and a precursor is obtained; centrifuging and drying the obtained precursor at 9000r/min and 75 ℃ for 11h, and calcining at 1000 ℃ for 2.5h to obtain BaFe 12 O 19 Nanoparticles；
Dissolving 2.5g zein and 1g ethylcellulose in 10mL 80% ethanol aqueous solution by volume to fill N 2 Bagging, carrying out irradiation modification, and separating out the modified zein fiber after the absorbed dose is 60 kGy;
1g of BaFe 12 O 19 The nano particles and 1g of modified Zein fiber are mixed and stirred for 30min, the mixture is put into a die after being uniformly dispersed, a film body with the thickness of 40mm multiplied by 1mm is formed by die casting, and magnetizing treatment is carried out under the strength of a 2T magnetic field, so that the BFO-Zein/EC magnetic film is obtained.
Comparative example 1
16.2g FeCl 3 ·6H 2 O and 1.465g BaCl 2 ·2H 2 O is dissolved in 100mL of deionized water, 10g of sodium hydroxide is added at 60 ℃ for continuous stirring for 4 hours, 2mL of oleic acid is added for continuous stirring for 1 hour, and a precursor is obtained; centrifuging and drying the obtained precursor at 5000r/min and 80 ℃ for 12 hours, and calcining at 900 ℃ for 2 hours to obtain BaFe 12 O 19 A nanoparticle;
2.5g zein was dissolved in 10mL of 70% strength by volume aqueous ethanol and N-charged 2 Bagging, carrying out irradiation modification, and separating out the modified zein fiber after the absorbed dose is 80 kGy;
2g of BaFe 12 O 19 Stirring the nano particles and 1g of modified Zein fiber for 30min, uniformly dispersing, placing into a die casting die to form a film body with the thickness of 40mm multiplied by 1mm, and carrying out magnetizing treatment to obtain the BFO-Zein magnetic film.
Comparative example 2
16.2g FeCl 3 ·6H 2 O and 1.465g BaCl 2 ·2H 2 O is dissolved in 100mL deionized water, 10g of sodium hydroxide is added at 60 ℃ for continuous stirring for 4 hours, 2mL of oleic acid is added for continuous stirring for 1 hour, and a precursor is obtained; centrifuging and drying the obtained precursor at 5000r/min and 80 ℃ for 12 hours, and calcining at 900 ℃ for 2 hours to obtain BaFe 12 O 19 Nanoparticles, noted BFO NPs.
The materials obtained in example 1 and comparative examples 1 to 2 were examined, and the results are shown in FIGS. 1 to 3.
As can be seen from fig. 1, BFO NPs have distinct characteristic diffraction peaks at 2θ=30.3, 32.2, 34.1, 37.1, 40.3, 42.4, 55.1, 56.3, 56.6, 63.1, corresponding to BaFe 12 O 19 A nanoparticle; the diffraction peak of the BFO-Zein/EC magnetic film obtained by the invention is very remarkable in the spectrum, which shows that the magnetic particles occupy a larger area in the magnetic film and have good magnetic force performance.
As can be seen from fig. 2, after the modification with oleic acid, the barium ferrite nano-particles have uniform size distribution and better dispersibility, the crystal phase is a flaky hexagonal crystal, the size range is between 50 and 200nm, and the size ranges from a single domain critical size (460 nm) to a superparamagnetic critical size (14 nm); the surface of the magnetic film is modified by using cellulose to form ridges of about 200nm, so that the material generates superhydrophobicity, the water stability of the film is greatly improved, and meanwhile, the 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 property compared with BFO-Zein magnetic film and BFO NPs.
As can be seen from FIG. 3, the saturation magnetization intensity of the BFO-Zein/EC magnetic film obtained by the invention is 44.75emu/g, the remanence is 24.84emu/g, and the coercivity is-4.8 k; the saturation magnetization intensity of BFO NPs is 65.19emu/g, the remanence is 33.32emu/g, and the coercivity is-4.8 k; the saturation magnetization intensity 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 property, but also has high stability, the magnetism can be kept stable for a long time, the film has obvious adsorption and aggregation effects on ferromagnetic particles, has positive significance on development of endogenous magnetic targeting, and can be used for in vivo sustained drug targeting of chronic diseases.
The foregoing is merely a preferred embodiment of the present invention and it should be noted that modifications and adaptations to those skilled in the art may be made without departing from the principles of the present invention, which are intended to be comprehended within the scope of the present invention.

Claims (9)

1. The preparation method of the 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, ethylcellulose and ethanol aqueous solution, and carrying out irradiation modification to obtain modified zein fibers;
s3: baFe is added to 12 O 19 Mixing the nano particles with modified Zein fibers, and magnetizing to obtain a BFO-Zein/EC magnetic composite film;
step S1 and step S2 have no sequence requirement;
in the step S2, the mass ratio of the zein to the ethylcellulose is 2-4: 1, the mass volume ratio of zein to ethanol aqueous solution is 1-3 g:10mL, the volume concentration of ethanol in the ethanol water solution is 60-80%.
2. The method for preparing the BFO-Zein/EC magnetic composite film material according to claim 1, wherein in the step S1, the mixing mode 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.
3. The method for preparing the BFO-Zein/EC magnetic composite film material according to claim 2, wherein in the 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 method for preparing the BFO-Zein/EC magnetic composite film material according to claim 3, wherein sodium hydroxide is added at 40-80 ℃ in the step S1.
5. The method for preparing the BFO-Zein/EC magnetic composite film material according to claim 1 or 2, wherein in the step S1, the calcination temperature is 700-1100 ℃ and the calcination time is 1-3 hours.
6. The method for preparing the BFO-Zein/EC magnetic composite film material according to claim 1, 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.
7. The method for preparing a BFO-Zein/EC magnetic composite film material according to any one of claims 1 to 4, wherein in step S3, baFe 12 O 19 The mass ratio of the nano particles to the modified zein fibers is 1-3: 1, a step of; before magnetizing, baFe 12 O 19 The mixture obtained by mixing the nano particles and the modified zein fibers is subjected to die casting molding; the intensity of the magnetized magnetic field is 0.5-5T.
8. The BFO-Zein/EC magnetic composite membrane material prepared by the method for preparing the BFO-Zein/EC magnetic composite membrane material according to any one of claims 1 to 7.
9. The use of the BFO-Zein/EC magnetic composite membrane material of claim 8 in the preparation of a magnetic drug.
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