CN109879326A - A method of ferric oxide nanometer particle is prepared using tealeaves - Google Patents
A method of ferric oxide nanometer particle is prepared using tealeaves Download PDFInfo
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- CN109879326A CN109879326A CN201910222894.1A CN201910222894A CN109879326A CN 109879326 A CN109879326 A CN 109879326A CN 201910222894 A CN201910222894 A CN 201910222894A CN 109879326 A CN109879326 A CN 109879326A
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- ferric oxide
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Abstract
The present invention discloses a kind of method for preparing ferric oxide nanometer particle using tealeaves, comprising the following steps: 1) iron hydrate is dissolved in tea extract, in N2Under protection, temperature is 60-100 DEG C, mixing speed is after the 20-40min that flows back, to add precipitating reagent under 900-1100rpm, and flow back 20-40min, then adds stabilizer, and flow back 50-70min, is cooled to room temperature, obtains black mixture；Iron hydrate is FeCl3•6H2O and FeCl2•4H2The mixture of O, stabilizer are citric acid；2) by the cleaning of step 1) black mixture, separation, ferric oxide nanometer particle is obtained.Citric acid is fixed on nano particle by the present invention by way of homogeneous reaction, overcome influence of the fixation support structural factor to nano particle immobilized rate in heterogeneous reaction, gained nano particle fixed rate is high, the immobilized reactant of citric acid and the reduction reaction substep of tea extract carry out, while citric acid immobilization, the molding of nano particle is also achieved, preparation process is simplified；Ferric oxide nanometer particle obtained has good monodispersity and cell compatibility.
Description
Technical field
The invention belongs to field of material technology, and in particular to a method of ferric oxide nanometer particle is prepared using tealeaves.
Background technique
Tealeaves refers to the leaf and bud of tea tree, is current active medicine most commonly used in the world, has good height water-soluble
The advantages of property, hypotoxicity and biocompatibility.Tea polyphenols (Tea Polyphenols) are that one kind that content is most in tealeaves is solvable
Property ingredient and tealeaves play one of main matter of its health care effect, such as: caffeine, theanine, tea saponin, fragrant camphor tree
Alcohol, catechin etc., and catechin can also remove the free radical of internal danger, prevent the development of various diseases.
Currently, researchers at home and abroad have developed a variety of methods to prepare ferric oxide nanometer particle, such as: high temperature thermal decomposition has
Machine metal precursor synthesizes height monodisperse ferric oxide nanometer particle, however, the ferric oxide nanometer particle of high temperature method preparation has
High hydrophobicity can only save in organic solvent, and greatly hinder the application of its biomedical aspect, especially in drug
In terms of sustained release, targeting-treatment of cancer.Although many ligand exchange processes provide hydrophily, water stability and magnetic for it
Field responsiveness is not effectively improved but.In order to improve its hydrocolloid stability, optional ligand is surface modified it,
Citric acid (Citric acid) is a kind of important organic acid, is rich in hydroxyl on strand, reacts, can make by the way that hydroxyl is fixed
It is fixed on ferric oxide nanometer particle.Ariya Saraswathy etc. is using citric acid as fixative, the ferric oxide nano of preparation
Particle high degree of dispersion in aqueous solution, and can keep stablizing [Biointerfaces.2014,117] for a long time in the solution.
Saumya Nigam etc. is also prepared as coating material having a size of 8-10 nm ferric oxide nanometer particles using citric acid, is passed through
Investment carrying medicament shows good cell compatibility [Journal of Magnetism and Magnetic
Materials 323 (2011) 237–243.].To sum up, the ferric oxide nanometer particle that existing preparation method is prepared
The defects of that there are biocompatibilities is lower, dimensional performance is difficult to control, to limit its application in biomedicine.
Summary of the invention
It is an object of that present invention to provide a kind of methods for preparing ferric oxide nanometer particle using tealeaves.
Based on above-mentioned purpose, the present invention takes following technical scheme:
A method of ferric oxide nanometer particle is prepared using tealeaves, comprising the following steps:
1) iron hydrate is dissolved in tea extract, in N2Under protection, temperature is 60-100 DEG C, mixing speed 900-
Under 1100rpm, after the 20-40min that flows back, precipitating reagent is added, flow back 20-40min, then adds stabilizer, and flow back 50-70min, cold
But to room temperature, black mixture is obtained；Iron hydrate is FeCl3•6H2O and FeCl2•4H2The mixture of O, stabilizer are citric acid；
2) by the cleaning of step 1) black mixture, separation, ferric oxide nanometer particle is obtained.
Tea extract is green tea Aqueous extracts, preparation method in step 1) are as follows: green tea is added to 90-100 DEG C of ultrapure water
In, it impregnates, is cooling, filtering, obtaining green tea Aqueous extracts；The usage ratio of green tea and ultrapure water is 2g ︰ 100mL.
In step 1), the concentration of citric acid is 2mg/mL, the dosage of iron hydrate, tea extract, precipitating reagent and citric acid
Than for (9-11) g ︰ (60-100) mL ︰ (15-25) mL ︰ (3-5) mL.
In step 1), FeCl3•6H2O and FeCl2•4H2The mass ratio of O is 7.39 ︰ 2.714.
In step 1), precipitating reagent is ammonium hydroxide.
In step 2, when cleaning, taking ultrapure water is cleaning agent；When separation, permanent magnet is taken to be separated.
Compared with prior art, the invention has the following advantages:
1, citric acid is fixed on nano particle by way of homogeneous reaction, overcomes fixation support in heterogeneous reaction
Influence of the structural factor to nano particle immobilized rate, gained nano particle fixed rate is high, the immobilized reactant and tea of citric acid
The reduction reaction substep of Aqueous extracts carries out, and while citric acid immobilization, also achieves the molding of nano particle, simplifies preparation
Process；Ferric oxide nanometer particle obtained has good monodispersity and cell compatibility；
2, green tea Aqueous extracts dissolved iron hydrate, it is process green, simple, it is from a wealth of sources and at low cost, tealeaves can also natural degradation,
With environment friendly；
3, preparation method is simple, reaction condition is mild, strong operability, and cost is relatively low, is conducive to industrialization promotion.
Detailed description of the invention
Fig. 1 is embodiment 1 and the XRD spectrum for comparing nano particle；
Fig. 2 is embodiment 1 and the FT-IR map for comparing nano particle；
Fig. 3 is embodiment 1 and the TEM picture for comparing nano particle；
Fig. 4 is embodiment 1 and the size distribution for comparing nano particle；
Fig. 5 is embodiment 1 and the zeta potential diagram for comparing nano particle；
Fig. 6 is DLS analysis of the nano particle of embodiment 1 in cell culture fluid.
Specific embodiment
FeCl3•6H2O、FeCl2•4H2O and citric acid are purchased from aldrich company (Aldrich, product batch number: 94676).
Green tea is Xinyang Maojian Tea, comes from Henan Province tea tree biology key lab.
Tea extract is green tea Aqueous extracts, preparation method in embodiment 1-3 are as follows: 2g green tea is added 100 DEG C of 100mL
Ultrapure water in, impregnate 30min, cooling, filtering obtains green tea Aqueous extracts.
Embodiment 1
A method of ferric oxide nanometer particle is prepared using tealeaves, comprising the following steps:
1) by 7.39g FeCl3•6H2O(4.44g FeCl3) and 2.714g FeCl2•4H2O(1.732g FeCl2) it is dissolved in 80
In mL tea extract, in N2Under protection, temperature is 70 DEG C, mixing speed is after the 30min that flows back, to add 20mL ammonia under 1000rpm
Water, flow back 30min, then adds 4mL 2mg/mL citric acid, and flow back 60min, is cooled to room temperature, obtains black mixture；
2) it takes ultrapure water to clean step 1) black mixture, permanent magnet is taken to be separated, obtain ferric oxide nano
Particle.
Embodiment 2
A method of ferric oxide nanometer particle is prepared using tealeaves, comprising the following steps:
1) by 7.39g FeCl3•6H2O(4.44g FeCl3) and 2.714g FeCl2•4H2O(1.732g FeCl2) it is dissolved in 80
In mL tea extract, in N2Under protection, temperature is 60 DEG C, mixing speed is after the 40min that flows back, to add 15mL ammonia under 900rpm
Water, flow back 40min, then adds 4mL 2mg/mL citric acid, and flow back 70min, is cooled to room temperature, obtains black mixture；
2) it takes ultrapure water to clean step 1) black mixture, permanent magnet is taken to be separated, obtain ferric oxide nano
Particle.
Embodiment 3
A method of ferric oxide nanometer particle is prepared using tealeaves, comprising the following steps:
1) by 7.39g FeCl3•6H2O(4.44g FeCl3) and 2.714g FeCl2•4H2O(1.732g FeCl2) it is dissolved in 80
In mL tea extract, in N2Under protection, temperature is 70 DEG C, mixing speed is after the 20min that flows back, to add 20mL ammonia under 1100rpm
Water, flow back 20min, then adds 5mL 2mg/mL citric acid, and flow back 50min, is cooled to room temperature, obtains black mixture；
2) it takes ultrapure water to clean step 1) black mixture, permanent magnet is taken to be separated, obtain ferric oxide nano
Particle.
4 performance measurement of embodiment
4.1 XRD, FT-IR and tem analysis
Ferric oxide nanometer particle made from embodiment 1 is known as T-C- nano particle.
The step of tea extract in embodiment 1 is changed to ultrapure water, lacks addition citric acid and reflux 60min, other
Condition is referred to as blank nano particle with embodiment 1, ferric oxide nanometer particle obtained.
The step of addition citric acid and reflux 60min will be lacked in embodiment 1, other conditions are the same as embodiment 1, oxygen obtained
Change iron nano-particle and is referred to as T- nano particle.
Tea extract in embodiment 1 is changed to ultrapure water, other conditions are the same as embodiment 1, ferric oxide nano obtained
Grain is referred to as C- nano particle.
To T-C- nano particle (T-C-SPION), blank nano particle (bare SPION), T- nano particle (T-
SPION), C- nano particle (C-SPION) carries out XRD, FT-IR and transmission electron microscope (TEM) analysis respectively, as a result distinguishes
As shown in Figure 1,2 and 3.
By Fig. 1 map it is found that T- nano particle and T-C- nano particle have higher crystallinity, T- nano particle exists
Peak value 2θ =25 ° show there is the active principle absorbed in green tea.
As shown in Figure 2, in 580 cm-1Peak value it is related with the vibration of iron oxygen key, this matches with the characteristic of iron oxide.?
3400 cm-1, O-H key is attached to the surface of nano particle, in 1710 cm of peak value-1Locate, C=O in the COOH group of citric acid
It is about 1600 cm in peak value in mal-distribution-1Place, C- nanoparticle pattern confirm that the acid group of citric acid passes through carboxylate
Particle is attached to the surface of nano particle.In 1637-1611 cm-1, absorb mainly C=C by containing in polyphenol compound
The stretching vibration of aromatic rings is dominated.In 1062 and 1044 cm-1Absorption band be C-O-C, the feature of O-H.Thus it demonstrate,proves
It is bright, the main plant chemical component in green tea include hydrophily catechin may be played during nano particle functionalization it is important
Effect, and it is further used as stabilizer, TEM picture also demonstrates the conclusion.
The monodisperse and spherical T-C- nano particle that diameter is 23.8 ± 0.8 nm, nano particle are observed by Fig. 3
Diameter is in the range of 15-40 nm, it is shown that superparamagnetism.In nano grain surface, the balance of lemon acid free radical and polyphenol
The dispersibility and stability of particle can be improved.And there is aggregation now in blank nano particle, T- nano particle, C- nano particle
As.
4.2 colloidal stabilities and cell compatibility detection
T-C- nano particle, blank nano particle, T- nanometers in 4.1 in deionized water (Millipore) are measured using DLS
Grain, the size distribution of C- nano particle and zeta current potential, result is respectively such as Figure 4 and 5.
It is learnt by Figure 4 and 5, compared with other samples, T-C- nano particle has preferable colloidal stability.
Cell compatibility test method:
1) cell suspension of 100 μ L is prepared in 96 orifice plates.By culture plate in incubator preculture 24 hours at 37 degree, 5% CO
Under conditions of.
2) sample material of 10 μ L various concentrations is added to culture plate.
3) culture plate is incubated for one section of reasonable time (6,12,24 or 48 hours) in incubator.
4) 10 μ LCCK-8 solution are added to every hole.
5) culture plate is incubated for 1-4 hours in incubator.
It is detected using CCK-8, as a result as shown in Figure 6.It is learnt by Fig. 6, T-C- nano particle is in cell culture medium
It has good stability, and stable preservation 6 weeks in water, without clustering phenomena.
In addition, CCK-8 test confirms that T-C- nano particle has good cell compatibility.It follows that system of the present invention
The T-C- nano particle obtained extends ferric oxide nanometer particle in the application of biomedical aspect.
The present invention prepares ferric oxide nanometer particle by tea extract and citric acid, has good monodispersity and cell
Compatibility is a kind of green synthesis method.
Claims (5)
1. a kind of method for preparing ferric oxide nanometer particle using tealeaves, which comprises the following steps:
1) iron hydrate is dissolved in tea extract, in N2Under protection, temperature is 60-100 DEG C, mixing speed 900-
Under 1100rpm, after the 20-40min that flows back, precipitating reagent is added, flow back 20-40min, then adds stabilizer, and flow back 50-70min, cold
But to room temperature, black mixture is obtained；Iron hydrate is FeCl3•6H2O and FeCl2•4H2The mixture of O, stabilizer are citric acid；
2) by the cleaning of step 1) black mixture, separation, ferric oxide nanometer particle is obtained.
2. the method for preparing ferric oxide nanometer particle using tealeaves as described in claim 1, which is characterized in that tea in step 1)
Aqueous extracts are green tea Aqueous extracts, preparation method are as follows: green tea are added in 90-100 DEG C of ultrapure water, impregnate, is cooling, filtering,
Obtain green tea Aqueous extracts；The usage ratio of green tea and ultrapure water is 2g ︰ 100mL
The method as claimed in claim 2 for preparing ferric oxide nanometer particle using tealeaves, which is characterized in that in step 1), lemon
The concentration of lemon acid is 2mg/mL, iron hydrate, tea extract, precipitating reagent and citric acid amount ratio be (9-11) g ︰ (60-100)
ML ︰ (15-25) mL ︰ (3-5) mL.
3. the method for preparing ferric oxide nanometer particle using tealeaves as claimed in claim 3, which is characterized in that in step 1),
FeCl3•6H2O and FeCl2•4H2The mass ratio of O is 7.39 ︰ 2.714.
4. the method for preparing ferric oxide nanometer particle using tealeaves as claimed in claim 4, which is characterized in that in step 1),
Precipitating reagent is ammonium hydroxide.
5. the method for preparing ferric oxide nanometer particle using tealeaves as described in claim 1, which is characterized in that in step 2,
When cleaning, taking ultrapure water is cleaning agent；When separation, permanent magnet is taken to be separated.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| KR20210062585A (en) * | 2019-11-21 | 2021-05-31 | 건국대학교 산학협력단 | Silica ferrite magnetic nanoparticles for the immobilization of enzyme, and preparation method thereof |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| KR20210062585A (en) * | 2019-11-21 | 2021-05-31 | 건국대학교 산학협력단 | Silica ferrite magnetic nanoparticles for the immobilization of enzyme, and preparation method thereof |
| KR102486631B1 (en) | 2019-11-21 | 2023-01-10 | 건국대학교 산학협력단 | Silica ferrite magnetic nanoparticles for the immobilization of enzyme, and preparation method thereof |
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