CN104949948B - A kind of magnetic flourescent nano material for magnetic and preparation method and application - Google Patents
A kind of magnetic flourescent nano material for magnetic and preparation method and application Download PDFInfo
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- CN104949948B CN104949948B CN201510342281.3A CN201510342281A CN104949948B CN 104949948 B CN104949948 B CN 104949948B CN 201510342281 A CN201510342281 A CN 201510342281A CN 104949948 B CN104949948 B CN 104949948B
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Abstract
The invention discloses a kind of magnetic flourescent nano material for magnetic and preparation method and application.The preparation method of the magnetic fluorescence nano trace particle, comprises the following steps：(1) ferroferric oxide magnetic nano-particles that surface modification is had to the coated with silica of carboxyl are scattered in dispersant, are added condensing agent and are activated；(2) fluorescein is added in step (1) system, after condensation reaction, collects solids with externally-applied magnetic field and produce the magnetic fluorescence nano trace particle.The magnetic flourescent nano material for magnetic can be used for the measure of feed mixture homogeneity.The preparation method of magnetic fluorescence nano trace particle of the present invention is simple, by process optimization, only needs a step just to can obtain；The magnetic fluorescence nano trace particle of the present invention, has the advantages that simple to operate, efficiency high, uniform particle diameter；Magnetic fluorescence nano trace particle of the present invention can be applied to the detection of feed mixture homogeneity, with higher detection efficiency and relatively low testing cost.
Description
Technical field
The present invention relates to a kind of magnetic flourescent nano material for magnetic and preparation method and application, more particularly to a kind of magnetic fluorescence
Nanometer trace particle and preparation method and application.
Background technology
Feed mixture homogeneity is evaluation feed mixing machine performance and the mostly important index of finished feed quality.But in reality
In the production of border, mixing does not often obtain everybody enough attention.The homogeneous feed of mixing is played for quality of the fodder control
Vital effect, and the growth of animal is directly affected, and then influence the overall economic benefit of cultivation.
Feed mixture homogeneity (CV%) only by determining, can just know whether and be up to state standards.Current industry pair
The CV values of mixture homogeneity are typically required：Mixed feed≤10%；Concentrated feed≤7%；Additive premix≤
5%.
The conventional methyl violet in the country, Chloride selective electrode method, methods for calcium, phosphorus determination method, methods for chlorides and thick
Albuminometry etc. determines feed mixture homogeneity.But above method meeting tested person reagent, the influence of feed ingredient, and use
Instrument is more, and operation is more complicated, and cost is higher.In recent years, the Magnetic Tracer particle method of functionalization is determining feed uniformity side
Face shows greater advantage.The Magnetic Tracer particle of wherein fluorescent functional is also rarely reported.
Nano-particle with magnetic and fluorescent dual-function is gathered around in bio-medical fields such as magnetic resonance imaging, biomarkers
There is wide application prospect.The syntheti c route of difference magnetic flourescent nano material for magnetic can be divided into following several at present：(1) with containing
The silicon dioxide layer of protection coated magnetic kernel of fluorescent material；(2) polymer protects magnetic kernel and glimmering in shell surface modification
Stimulative substance；(3) ion with magnetic kernel and fluoride ions compound shell is prepared by the interaction of positive and negative charge to gather
Collective；(4) magnetic Nano kernel direct covalent bonds close fluorescent material etc..
The content of the invention
It is an object of the invention to provide a kind of magnetic flourescent nano material for magnetic and preparation method and application, the preparation method with
Surface modification has the ferroferric oxide magnetic nano-particles (Fe of the coated with silica of carboxyl3O4@SiO2- COOH) it is main former
Material, using the carboxyl on its surface, is connected with the fluorescein of amino by surface and is fixed on the nano-particle, and surface work is carried out to material
Energyization is modified, so that the nano-particle has fluorescence and magnetic simultaneously, simple to operate, with low cost, the magnetic prepared is glimmering
Light nano material can be used for the on-line checking of feed mixing degree.
The invention provides a kind of preparation method of magnetic fluorescence nano trace particle, comprise the following steps：
(1) ferroferric oxide magnetic nano-particles that surface modification is had to the coated with silica of carboxyl are scattered in dispersant
In, add condensing agent and activated；
(2) fluorescein is added in step (1) system, after condensation reaction, collecting solids with externally-applied magnetic field is
Obtain the magnetic fluorescence nano trace particle.
In above-mentioned preparation method, in step (1), the every 200~500mg nano-particle is dispersed among 50~
In dispersant described in 125mL, concretely following 1) -5) it is any in：
1) nano-particle described in every 200~400mg is scattered in dispersant described in 50~100mL；
2) the every 400~500mg nano-particle is scattered in dispersant described in 100~125mL；
3) nano-particle per 200mg is scattered in dispersant described in 50mL；
4) nano-particle per 400mg is scattered in dispersant described in 100mL；
5) nano-particle per 500mg is scattered in dispersant described in 125mL.
The dispersant can be dichloromethane, N, in N '-dimethyl formamide (DMF) and dimethyl adipate (DMA)
It is at least one.
In above-mentioned preparation method, in step (1), the mass ratio of the condensing agent and the nano-particle can be 3：(1.5
~5), concretely 3：4；
The condensing agent can be 2- (7- azos BTA)-N, N, N', N'- tetramethylurea hexafluorophosphoric acids ester, benzo
Triazole-N, N, N', N'- tetramethylurea hexafluorophosphoric acid ester, n-hydroxysuccinimide, N, N'- Dicyclohexylcarbodiimides, 1-
(3- dimethylamino-propyls) at least one of -3- ethyl-carbodiimide hydrochlorides and N, N'- DIC, specifically may be used
For n-hydroxysuccinimide and 1- (3- dimethylamino-propyls) -3- ethyl-carbodiimide hydrochlorides；
The n-hydroxysuccinimide (condensing agent A) and the 1- (3- dimethylamino-propyls) -3- ethyl carbodiimides
The mass ratio of hydrochloride (condensing agent B) can be 1：(1~4), concretely 1：2；
The mass ratio of i.e. described condensing agent A, the condensing agent B and the nano-particle can be 1：2：(1.5~5), specifically
Can be 1：2：4.
It is as follows the step of the activation in above-mentioned preparation method, step (1)：PH to 4~6, stirring are adjusted with watery hydrochloric acid
2~2.5h of ultrasound is completely dissolved to the condensing agent.
In above-mentioned preparation method, step (2), the fluorescein can for DAP, N- aryl -4- amino -
1,8- benzene-naphthalene diimides, 2,7- dichloro isothiocyanates fluorescein, 5- Aminofluoresceins, 2,7- dichloros Aminofluorescein and 5- are different
At least one of thiocyanates fluorescein, concretely DAP, N- aryl -4- amino -1,8- benzene-naphthalene diimide,
2,7- dichloro isothiocyanates fluorescein, 5- Aminofluoresceins, 2,7- dichloros Aminofluorescein and 5- isothiocyanates fluoresceins
Any of；
The addition of the fluorescein and the nano-particle (Fe3O4@SiO2- COOH) mass ratio can be 1：(0.5~
5), concretely 1：1.
In above-mentioned preparation method, step (2), the condensation reaction is carried out under agitation, and temperature can be 20~35
DEG C, concretely 25 DEG C；Time can be 10~16h, concretely 10~14h, 14~16h, 10h, 14h or 16h.
Also include the magnetic fluorescence nano trace particle is washed and done after above-mentioned preparation method, step (2)
Dry step；
The drying can be vacuum drying, and temperature can be 20~35 DEG C, concretely 25 DEG C；Time can be 12~24h, tool
Body can be 12~18h, 18~24h, 12h, 18h or 24h.
Present invention provides the magnetic fluorescence nano trace particle that a kind of above-mentioned preparation method is prepared, pass through scanning
The means such as Electronic Speculum (SEM), vibrating specimen magnetometer (VSM), X-ray diffraction (XRD), FTIR spectrum (FTIR) are entered to it
Sign is gone.
Surveyed invention further provides the magnetic fluorescence nano trace particle that a kind of above-mentioned preparation method is prepared
Determine the application in feed mixture homogeneity.
Magnetic fluorescence nano trace particle of the present invention is added in feed, its rate of recovery up to 90.2%~93.5%, because
This, can utilize its fluorescent characteristic, and magnetic fluorescence nano trace particle of the present invention is applied into the well mixed of on-line checking feed
Degree.
In above-mentioned application, the step of determining feed mixture homogeneity using magnetic fluorescence nano trace particle of the present invention is such as
Under：
(1) foundation of standard curve：The fluorescence for determining the magnetic fluorescence nano trace particle of at least three kinds various concentrations is strong
Degree, sets up the concentration of the magnetic fluorescence nano trace particle and the standard curve of fluorescence intensity；
(2) measure of feed mixture homogeneity：After the magnetic fluorescence nano trace particle is mixed with feed to be measured, take
Go out at least 10 parts biased samples, the magnetic fluorescence nano trace particle is isolated from the testing sample with externally-applied magnetic field
Come, detect its fluorescence intensity respectively with sepectrophotofluorometer, the magnetic fluorescence nano spike is obtained according to the standard curve
The quality of particle, analysis calculates the coefficient of variation (CV%) of the sample, you can the mixture homogeneity of the reflection feed.
In said determination method, in step (1), in the standard curve, the magnetic fluorescence nano trace particle it is dense
Spend for 1.0~6.0mg/mL.
In said determination method, in step (2), the 2~5mg magnetic fluorescence nano is added in feed described in per 10g
Trace particle, concretely adds magnetic fluorescence nano trace particle described in 250.0mg in feed described in every 60.0g.
In said determination method, the feed can be any of concentrate feed, premix and mixed feed.
The present invention has the advantages that：
(1) present invention is with nanometer Fe3O4For magnetic kernel, surface protection is carried out to it with silica, makes material more steady
Qualitative and resistance to acids and bases, and using the carboxylic-bond fluorescence molecule on surface, fluorescence molecule is grafted with magnetic particle more firm, make
Material has fluorescence and magnetic concurrently.By process optimization, a step is only needed just to can obtain performance stabilization, the magnetic having wide range of applications
Fluorescence nano trace particle.
(2) magnetic fluorescence nano trace particle of the invention, has the advantages that simple to operate, efficiency high, uniform particle diameter, and
It is applied to the detection of feed mixture homogeneity, higher detection efficiency and relatively low testing cost can be reached.
Brief description of the drawings
Fig. 1 is the preparation flow schematic diagram of magnetic fluorescence nano trace particle of the present invention.
Fig. 2 is ESEM (SEM) photo of the magnetic fluorescence nano trace particle prepared in embodiment 1.
Fig. 3 is the hysteresis curve (VSM) of the magnetic fluorescence nano trace particle prepared in embodiment 1.
Fig. 4 is the infrared spectrum (IR) of the magnetic fluorescence nano trace particle prepared in embodiment 1.
Fig. 5 is the x-ray diffraction pattern (XRD) of the magnetic fluorescence nano trace particle prepared in embodiment 1.
Fig. 6 is magnetic fluorescence nano trace particle Standardization curve for fluorescence intensity figure in embodiment 5.
Embodiment
Experimental method used in following embodiments is conventional method unless otherwise specified.
Material, reagent used etc., unless otherwise specified, are commercially obtained in following embodiments.
Tester and condition in following embodiments：Super-resolution cold field emission SEM：FDAC
(Hitachi) company SU8020 types；Superconductive quantum interference magnetometer：Quantum Design companies of U.S. MPMS-XL-7 types；X-
X ray diffractometer x：German Brooker (Bruker) company D8Advance types；Fourier infrared spectrograph：U.S. Buddhist nun high-tensile strength
(Nicolet) types of instrument company Magna-IR 170；Sepectrophotofluorometer：PerkinElmer instrument (Shanghai) Co., Ltd.
LS55 types.
Raw material surface in following embodiments used in preparation process is modified with the core shell structure ferroso-ferric oxide of carboxyl
Magnetic nano-particle (Fe3O4@SiO2- COOH) nanometer Science and Technology Ltd. of Wenzhou peace section is purchased from, specification is 500nm.
Embodiment 1, prepare magnetic fluorescence nano trace particle
Magnetic Nano trace particle, schematic flow sheet as shown in Figure 1 are prepared as steps described below：
(1) the core shell structure ferroferric oxide magnetic nano grain (Fe of surface modification carboxyl is taken3O4@SiO2-COOH)
200.0mg ultrasonic disperses are in 50.0mL N, N '-dimethyl formamide, after solution is homogeneous, add 50.0mg N- hydroxyl ambers
Amber acid imide (NHS) and 100.0mg ethyl carbodiimides (EDC), pH to 4 is adjusted with watery hydrochloric acid, and stirring 2h is simultaneously ultrasonic to complete
Fully dissolved.
At (2) 25 DEG C, in step (1) system, add stirring 10h after 200.0mg 5- Aminofluoresceins and reacted.
After completion of the reaction, magnetic particle is collected with additional magnet, is washed twice respectively with deionized water, ethanol, is dried in vacuo at 25 DEG C
12h, you can obtain magnetic Nano trace particle.
Embodiment 2, prepare magnetic fluorescence nano trace particle
Magnetic Nano trace particle, schematic flow sheet as shown in Figure 1 are prepared as steps described below：
(1) the core shell structure ferroferric oxide magnetic nano-particles (Fe of surface modification carboxyl is taken3O4@SiO2-COOH)
400.0mg ultrasonic disperses are in 100.0mL N, N '-dimethyl formamide, after solution is homogeneous, add 100.0mg NHS and
200.0mg EDC, pH to 5 is adjusted with watery hydrochloric acid, stirring 2.5h simultaneously ultrasound to being completely dissolved.
At (2) 25 DEG C, in step (1) system, add stirring 14h after 400.0mg 5- Aminofluoresceins and reacted.
After completion of the reaction, with solids in additional magnet collection system, washed twice respectively with deionized water, ethanol, it is true at 25 DEG C
Sky dries 18h, you can obtain magnetic Nano trace particle.
Embodiment 3, prepare magnetic fluorescence nano trace particle
Magnetic Nano trace particle, schematic flow sheet as shown in Figure 1 are prepared as steps described below：
(1) the core shell structure ferroferric oxide magnetic nano-particles (Fe of surface modification carboxyl is taken3O4@SiO2-COOH)
500.0mg ultrasonic disperses are in 125.0mL N, N '-dimethyl formamide, after solution is homogeneous, add 125.0mg N- hydroxyls
Succinimide (NHS) and 250.0mg ethyl carbodiimides (EDC), pH to 6, stirring 2.5h and ultrasound are adjusted with watery hydrochloric acid.
At (2) 25 DEG C, in step (1) system, add stirring 16h after 500.0mg 5- Aminofluoresceins and reacted.
After completion of the reaction, with solids in additional magnet collection system, washed twice respectively with deionized water, ethanol, it is true at 25 DEG C
Sky dries 24h, you can obtain magnetic Nano trace particle.
The sign of embodiment 4, magnetic fluorescence nano trace particle
Fig. 2 is the stereoscan photograph of the magnetic Nano trace particle prepared in embodiment 1, as seen from Figure 2,
Though nano particle overlaps, essentially individual layer, product is spherical in shape, and average grain diameter is~500nm, the bumps of material surface
Structure is the fluorescence molecule of grafting.The magnetic Nano trace particle prepared in other embodiments of the present invention is without significant difference.
Fig. 3 is the hysteresis curve for the magnetic Nano trace particle that embodiment 1 is prepared, and as seen from Figure 3, magnetic is received
The saturation magnetization of rice trace particle material is~13emu/g, and magnetic response is good, and good point can be realized under magnetic field
From.The saturation magnetization for the magnetic Nano trace particle that embodiment 2 and embodiment 3 are prepared is same as Example 1, is
13emu/g。
In the infrared spectrum for the magnetic Nano trace particle that Fig. 4 prepares for embodiment 1, Fig. 4,3430cm-1Locate as 5-
- OH characteristic absorption peak in Aminofluorescein molecule；1633cm-1Locate the characteristic absorption peak for amido link, illustrate magnetic core surface
Carboxyl there occurs condensation reaction with the amino in fluorescence molecule；1089cm-1Locate for the characteristic absorption peak of Si-O keys, to illustrate magnetic core
There is silica protection shell in surface, these characteristic peaks show that successfully magnetic nano-particle has been arrived in modification to fluorescein molecule
Surface, and the structure of former magnetic nano-particle keeps constant.The infrared spectrum that other embodiments of the present invention are prepared goes out
Features described above peak is showed, has shown that fluorescein molecule of the present invention successfully modifies the surface for having arrived magnetic ion, and structural integrity.
In the magnetic Nano trace particle X-ray diffracting spectrum that Fig. 5 prepares for embodiment 1, Fig. 5, Fe is occurred in that3O4
6 typical 2 θ angles be located at 30.2 °, 35.6 °, 43.2 °, 53.4 °, 57.1 ° and 62.9 ° of absworption peak, correspond respectively to
Fe3O4In (220), (311), (400), (422), the absorption of (511) and (440) illustrates Fe3O4The presence of crystal structure.It is real
The X-ray diffracting spectrum and the collection of illustrative plates of the magnetic Nano trace particle that example 2 and embodiment 3 are prepared are applied without substantive difference.
The application of embodiment 5, magnetic fluorescence nano trace particle in feed mixture homogeneity is determined
(1) measure of magnetic fluorescence nano trace particle rate of recovery in feed
The magnetic fluorescence nano trace particle that embodiment 2 is prepared, be configured to a series of concentration knowns (1mg/mL,
2mg/mL, 4mg/mL, 5mg/mL and 6mg/mL) magnetic fluorescent nanometer particle standard liquid, according to by dilute to dense order, survey
Determine the fluorescence intensity of standard liquid, draw the working curve of concentration-fluorescence intensity, see Fig. 6.The maximum excitation of fluoroscopic examination condition
Wavelength 492nm, maximum emission wavelength 518nm, slit width is 2.5nm.The range of linearity is between 1.0~6.0mg/mL, linearly
Equation is Y=1.681x+0.0.Coefficient correlation is 0.9982.
Concentrate feed, premix and each 10.00 ± 0.01g of batch are weighed respectively, and 50.0mg implementations are separately added into thereto
The magnetic fluorescence nano trace particle prepared in example 2, externally-applied magnetic field (magnet) is used to spike after uniform mixing in bottom
Particle is separated, and is had magnetic trace particle and is stayed in template surface, collects, quantitative dilute with 12.0mL deionized waters
Release, upper machine determines fluorescence intensity, every kind of feed is repeated three times, tries to achieve average value, the dense of the solution is obtained by working curve
Contain magnetic fluorescence tracer quality in degree and solution, calculate the rate of recovery for obtaining trace particle, the results are shown in Table 1.
Table 1, magnetic fluorescence nano trace particle detect the rate of recovery of feed mixing degree
As can be seen from Table 1, when magnetic fluorescence nano trace particle of the present invention being used to detect feed mixture homogeneity, its
The rate of recovery is between 90.2%-93.5%.
(2) magnetic fluorescence nano trace particle on-line checking feed mixture homogeneity
The magnetic prepared in 250.0mg above-described embodiments 3 is added in 60.0g concentrate feeds, premix and mixed feed respectively
Property fluorescence nano trace particle, after both fully mix, in every kind of feed sample ten parts, every part of 5.00 ± 0.01g is utilized respectively
Externally-applied magnetic field collects magnetic fluorescence nano trace particle therein, and using 5.0mL deionized water dissolvings, it is strong that upper machine determines its fluorescence
Degree, the quality of wherein trace particle is calculated according to calibration curve equation, so as to calculate trace particle quality in ten parts of samples
Average value A, standard deviation S and coefficient of variation CV (%), as a result as shown in table 2.
The mixture homogeneity result of the magnetic fluorescence nano trace particle on-line checking Three feed of table 2
As can be seen from Table 2, magnetic fluorescence nano trace particle of the present invention is used to detecting that feed to be (including batch, dense
Contracting material and premix) mixture homogeneity when, its coefficient of variation is between 4.8%-5.9%.
The embodiment above is the description of the invention and cannot be used for the limitation present invention, with claims of the present invention
Any change in suitable implication and scope, is all considered as being included within the scope of the claims.
Claims (7)
1. a kind of method that utilization magnetic fluorescence nano trace particle determines feed mixture homogeneity, comprises the following steps：
(1) foundation of standard curve：The fluorescence intensity of the magnetic fluorescence nano trace particle of at least three kinds various concentrations is determined, is built
Found the concentration of the magnetic fluorescence nano trace particle and the standard curve of fluorescence intensity；
The magnetic fluorescence nano trace particle is prepared according to the method comprised the following steps：
1) ferroferric oxide magnetic nano-particles that surface modification is had to the coated with silica of carboxyl are scattered in dispersant, plus
Enter condensing agent to be activated；
2) in step 1) add fluorescein in system, after condensation reaction, collected with externally-applied magnetic field solids produce it is described
Magnetic fluorescence nano trace particle；
(2) measure of feed mixture homogeneity：After the magnetic fluorescence nano trace particle is mixed with feed to be measured, take out extremely
Few 10 parts of biased samples, separate the magnetic fluorescence nano trace particle from the testing sample with externally-applied magnetic field,
Detect its fluorescence intensity respectively with sepectrophotofluorometer, the magnetic fluorescence nano trace particle is obtained according to the standard curve
Quality, analysis calculates the coefficient of variation of the testing sample, you can the mixture homogeneity of the reflection feed.
2. according to the method described in claim 1, it is characterised in that：2~5mg the magnetic is added in feed described in per 10g
Fluorescence nano trace particle；
The feed is any of concentrate feed, premix and mixed feed.
3. method according to claim 1 or 2, it is characterised in that：Step (1) 1) in, the described of every 200~500mg receives
Rice corpuscles is scattered in dispersant described in 50~125mL；
The dispersant is dichloromethane, N, at least one of N'- dimethylformamides and dimethyl adipate；
The mass ratio of the condensing agent and the nano-particle can be 3：(1.5~5)；
The condensing agent be 2- (7- azos BTA)-N, N, N', N'- tetramethylurea hexafluorophosphoric acids ester, BTA-
N, N, N', N'- tetramethylurea hexafluorophosphoric acid ester, n-hydroxysuccinimide, N, N'- Dicyclohexylcarbodiimides, 1- (3- diformazans
At least one of aminopropyl) -3- ethyl-carbodiimide hydrochlorides and N, N '-DIC.
4. method according to claim 3, it is characterised in that：Step (1) 1) in, the condensing agent is N- hydroxysuccinimidyl acyls
Imines and 1- (3- dimethylamino-propyls) -3- ethyl-carbodiimide hydrochlorides；
The mass ratio of the n-hydroxysuccinimide and the 1- (3- dimethylamino-propyls) -3- ethyl-carbodiimide hydrochlorides
Can be 1：(1~4).
5. method according to claim 4, it is characterised in that：Step (1) 1) in, it is as follows the step of the activation：With dilute
Salt acid for adjusting pH is to 4~6, and stirring 2~2.5h of ultrasound to the condensing agent is completely dissolved.
6. method according to claim 5, it is characterised in that：Step (1) 2) in, the fluorescein is 2,6- diaminourea pyrroles
Pyridine, N- aryl -4- amino -1,8- benzene-naphthalene diimides, 2,7- dichloro isothiocyanates fluorescein, 5- Aminofluoresceins, 2,7- bis-
At least one of chloro amido fluorescein and 5- isothiocyanates fluoresceins；
The mass ratio of the addition of the fluorescein and the nano-particle is 1：(0.5~5).
7. method according to claim 6, it is characterised in that：Step (1) 2) in, the condensation reaction is under agitation
Carry out, temperature is 20~35 DEG C, the time is 10~16h.
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| CN105067539A (en) * | 2015-07-16 | 2015-11-18 | 浙江大学 | Method for detecting mixing uniformity of soil heavy metal pollution samples |
| CN105826805B (en) * | 2016-05-24 | 2023-12-19 | 中国计量大学 | Random fiber laser capable of being magnetically regulated and controlled |
| CN109282963A (en) * | 2018-09-21 | 2019-01-29 | 北京理工大学 | Multimedium tracing method based on magnetic fluorescent particles |
| CN109913202A (en) * | 2019-04-26 | 2019-06-21 | 中国烟草总公司郑州烟草研究院 | A kind of preparation method and application of fluorescence nano carbon particle |
| CN112304998A (en) * | 2020-08-20 | 2021-02-02 | 成都理工大学 | Shale pore structure fluid flow channel tracer, preparation method and tracing method |
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