CN105400517B - Detect difunctional magnetic fluorescence probe preparation method and its application of cadmium ion - Google Patents
Detect difunctional magnetic fluorescence probe preparation method and its application of cadmium ion Download PDFInfo
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- CN105400517B CN105400517B CN201510728313.3A CN201510728313A CN105400517B CN 105400517 B CN105400517 B CN 105400517B CN 201510728313 A CN201510728313 A CN 201510728313A CN 105400517 B CN105400517 B CN 105400517B
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Abstract
The invention discloses a kind of difunctional magnetic fluorescence probe for detecting cadmium ion and preparation method thereof, magnetic fluorescent microspheres of the method using CdTe/CdS quantum dots and with superparamagnetism carry out the difunctional magnetic fluorescence probe of chemical reactive synthesis as material under the conditions of alkalescence, low temperature, darkness.The preparation method of the present invention is quick, easy, sensitivity is good, and difunctional magnetic fluorescence probe size tunable, fluorescence intensity height, the good dispersion synthesized, has the characteristics of magnetic microsphere Magnetic Isolation, can be recycled, can be recycled.The detection of heavy metal cadmium ion is carried out using the difunctional magnetic fluorescence probe of the present invention, there is the advantages of quick, easy, sensitive, be adapted to marketing application.
Description
Technical field
The invention belongs to detection of heavy metal ion field, more particularly to a kind of difunctional magnetic fluorescence for detecting cadmium ion to visit
Pin preparation method and applications.
Background technology
Developing rapidly for the modernization of industry and constantly bringing forth new ideas for Chemical Engineering Technology, cadmium is widely used in Chemical Manufacture,
But as cadmium usage amount constantly increases, the pollution caused by cadmium starts to attract people's attention.Cadmium ion is in heavy metal pollution
One of pollution sources of most serious, its caused toxic hazard are much larger than other metallic pollutions, and it not only cannot be by raw on the earth
Object is degraded, and by other chemical actions such as enrichments, can be directly or indirectly to the Nature biology and the health of the mankind
Threaten.The traditional detection method of heavy metal ion is varied, and in environment measuring, the method for detecting cadmium ion is main
Have：Electrochemical methods, graphite oven atomic absorption, ultraviolet spectrophotometry, anodic stripping voltammetry, atomic absorption spectrum
Method, inductively coupled plasma mass spectrometry etc., though these methods can carry out certain analysis and measure to cadmium ion, can not yet
Cadmium ion content with degree is measured, but their most complex operations, sample treatment are troublesome, need large-scale instrument, are parsed into
This height, analysis time length, and when interfering ion is more, error is big, has a strong impact on the accuracy of measurement result, while some are detected
Complex steps, be not suitable for the analysis and detection of site environment, it is difficult to popularization and application.
Semiconductor-quantum-point turns into star's material of nearest materials science field, it has because of its excellent performance
Excitation wavelength range is wider, and distribution is continuous, and emission peak is narrower, and is symmetric, overlapping smaller each other, it is not easy to mutually dry
Disturb, yield is higher, good light stability, and anti-light bleaching power is strong, and fluorescence lifetime is grown, and has good spatial compatibility etc. excellent
Point, wide application prospect is presented in the field such as ion measurement, bioprobe, cell marking and imaging, drug monitoring.
Fluorescent microsphere refers to that diameter in nanoscale to micro-scaled range, is loaded with fluorescent material, stimulated by outside energy
The solia particle of fluorescence can be inspired.Its profile can be arbitrary shape, and representative configuration is spherical.Detection of heavy metal ion at present
Study hotspot is to improve the sensitivity of biological detection and amplifies detection signal, and fluorescent microsphere is as a kind of new, tool
There is the fluorescent material of special light, electricity, magnetic property, be also widely used in bio-imaging, biological detection and ion measurement etc..
The content of the invention
It is simple and convenient to operate the technical problem to be solved in the present invention is to provide a kind of technics comparing and efficiently detects cadmium ion
Difunctional magnetic fluorescence probe preparation method and its application, the difunctional magnetic fluorescence probe pin fluorescence intensity of gained it is high, scattered
Property it is good and there is the characteristics of magnetic microsphere Magnetic Isolation, can be recycled.
In order to solve the above technical problems, the present invention uses following technical scheme：Detect the difunctional magnetic fluorescence of cadmium ion
Probe preparation method, using CdTe/CdS quantum dots and with superparamagnetism magnetic fluorescent microspheres as material, alkalescence, low temperature,
The difunctional magnetic fluorescence probe of chemical reactive synthesis is carried out under the conditions of darkness.
The difunctional magnetic fluorescence probe preparation method of above-mentioned detection cadmium ion, comprises the following steps：
(1) CdTe/CdS quantum dots are synthesized
Using one kettle way Hydrothermal Synthesiss CdTe/CdS quantum dots；100mL redistilled waters are added in three-neck flask, are added
After caddy, stirring sequentially adds trisodium citrate, mercaptopropionic acid, is stirred until homogeneous to dissolving；Then, it is molten with sodium hydroxide
Liquid adjusts pH；Then sodium tellurite, sodium borohydride, stirring to dissolving are separately added into；Finally, magneton is put into, flask is placed in magnetic
In power agitator, condenser pipe, 90 DEG C of oil bath heatings are loaded onto；During red light quantum point to be obtained, you can take out；
Then, CdTe/CdS quantum dot solutions are purified, the quantum dot aqueous solution of synthesis is cooled to room temperature, takes 5-
7mL quantum dot, the absolute ethyl alcohol of 2 times of volumes is added, is centrifuged using supercentrifuge, removes supernatant after centrifugation, lower floor sinks
Form sediment and dissolved with 5-7mL redistilled water, it is standby；
(2) difunctional magnetic fluorescence probe is synthesized
Weigh that 2mg EDC is soluble in water, add in the quantum dot purification liquid obtained by step (1), stir after dissolving,
It is activated, pH is adjusted with hydrochloric acid solution, then stirs 30min, it is standby；
Take 100 μ L, 5mg/ml magnetic fluorescent microspheres to be placed in 10ml PE pipes, add distilled water diluting to 5-7ml, ultrasonic wave
After scattered, magnetic fluorescent microspheres are mixed with the solution of above-mentioned gained, stirred, then adjust pH with sodium hydroxide solution,
It is eventually adding magneton to be placed on magnetic stirring apparatus, sample is reacted in 4 DEG C of dark condition；After reaction terminates, it is centrifuged repeatedly,
Remove unreacted quantum dot in supernatant, until the fluorescence of supernatant no longer reduces, the magnetic fluorescence probe that will be obtained
It is dissolved in distilled water, produces difunctional magnetic fluorescence probe.
In step (1), the quality of caddy is 0.1~0.2g, and trisodium citrate is 0.2~0.3g, mercaptopropionic acid 50
~70 μ L, pH to 11, sodium tellurite 0.02g, sodium borohydride 0.1g are adjusted with sodium hydroxide；Centrifuge speed reaches during centrifugation
To 5000r/min.
Hydrochloric acid conditioning solution pH to 6 is used in step (2), with sodium hydrate regulator solution pH to 8~9, the moon of sample at 4 DEG C
Reacted 12 hours in dark situation.
Magnetic fluorescent microspheres in step (2) are 500nm amino-magnetic microballoons.
The difunctional magnetic fluorescence probe that above-mentioned preparation method obtains.
Application of the above-mentioned difunctional magnetic fluorescence probe in cadmium ion is detected.
The problem of expensive, operation is complicated, the time is tediously long be present for traditional heavy metal cadmium ion detection, based on magnetic
Microballoon has the characteristics of good fluorescence property, inventor devise a kind of difunctional magnetic fluorescence probe for detecting cadmium ion and its
Preparation method, the method using CdTe/CdS quantum dots and with superparamagnetism magnetic fluorescent microspheres as material, alkalescence, low temperature,
The difunctional magnetic fluorescence probe of chemical reactive synthesis is carried out under the conditions of darkness.The preparation method of the present invention is quick, easy, sensitivity
Difunctional magnetic fluorescence probe size tunable, fluorescence intensity height, good dispersion good, and synthesize, have magnetic microsphere magnetic point
From the characteristics of, can be recycled, can be recycled.Heavy metal is carried out using the difunctional magnetic fluorescence probe of the present invention
The detection of cadmium ion, there is the advantages of quick, easy, sensitive, be adapted to marketing application.
Brief description of the drawings
Fig. 1 is the ultraviolet-visible absorption spectroscopy of magnetic microsphere (a), difunctional magnetic fluorescence probe (b) and quantum dot (c).
Fig. 2 is the fluorescence spectrum of quantum dot (a) and difunctional magnetic fluorescence probe (b).
Fig. 3 be difunctional magnetic fluorescence probe under white light under (left side) and uviol lamp (right side) image.
Fig. 4 is the electron microscope of difunctional magnetic fluorescence probe.
Fig. 5 is the partial enlarged drawing of difunctional magnetic fluorescence probe.
Fig. 6 is difunctional magnetic fluorescence probe electron scattering energy spectrum diagram.
Fig. 7 is cadmium ion detection method phenogram.
Fig. 8 is influence figure of the different EDTA concentration to system fluorescence.
Fig. 9 is concentration of cadmium ions and the variation diagram of fluorescence intensity.
Figure 10 is the working curve of cadmium ion measure.
Embodiment
First, the preparation of difunctional magnetic fluorescence probe
Using CdTe/CdS quantum dots and the magnetic fluorescent microspheres with superparamagnetism is materials, in alkalescence, low temperature, dark bar
Chemical reactive synthesis is carried out under part, specifically includes following steps：
(1) CdTe/CdS quantum dots are synthesized
Using one kettle way Hydrothermal Synthesiss CdTe/CdS quantum dots；100mL redistilled waters are added in three-neck flask, are added
After 0.1~0.2g of caddy, stirring sequentially adds 0.2~0.3g of trisodium citrate, the μ of mercaptopropionic acid (MPA) 50~70 to dissolving
L, it is stirred until homogeneous；Then, then it is separately added into sodium tellurite with the sodium hydroxide solution regulation pH to 11 or so of existing preparation
0.02g, sodium borohydride 0.1g, stirring to dissolving；Finally, magneton is put into, flask is placed in magnetic stirring apparatus, loads onto condensation
Pipe, 90 DEG C of oil bath heatings；During red light quantum point to be obtained, you can take out；
Then, CdTe/CdS quantum dot solutions are purified, the quantum dot aqueous solution of synthesis is cooled to room temperature, takes 5-
7mL quantum dot, add 2 times of volumes absolute ethyl alcohol, centrifuged (5000r/min) using supercentrifuge, remove after centrifugation on
Clear liquid, lower sediment 5-7mL redistilled water dissolves, standby；
(2) difunctional magnetic fluorescence probe is synthesized
Weigh that 2mg EDC is soluble in water, add in the quantum dot purification liquid obtained by step (1), stir after dissolving,
It is activated, pH to 6 or so is adjusted with hydrochloric acid solution, then stirs 30min, it is standby；
Take 100 μ L, 5mg/ml magnetic fluorescent microspheres to be placed in 10ml PE pipes, add distilled water diluting to 5-7ml, ultrasonic wave
After scattered, magnetic fluorescent microspheres are mixed with the solution of above-mentioned gained, stirred, then with sodium hydroxide solution regulation pH to
8~9, it is eventually adding magneton and is placed on magnetic stirring apparatus, sample is reacted 12 hours in 4 DEG C of dark condition；Reaction terminates
Afterwards, it is centrifuged repeatedly, removes unreacted quantum dot in supernatant, until the fluorescence of supernatant no longer reduces, by what is obtains
Magnetic fluorescence probe is dissolved in distilled water, produces difunctional magnetic fluorescence probe.
As shown in Figures 1 to 6, ultra-violet absorption spectrum (Fig. 1), fluorescence light are carried out by the difunctional magnetic fluorescence probe of preparation
Compose (Fig. 2) and (Fig. 3) is contrasted under white light and uviol lamp and characterize, can prove that quantum dot is successfully adsorbed on magnetic microsphere, have
Have stronger fluorescence intensity, can Magnetic Isolation, and during synthesizing magnetic fluorescence probe, quantum dot is not rolled into a ball
Poly-, dispersiveness is preferably.
Characterized by Electronic Speculum (Fig. 4, Fig. 5) and electron scattering power spectrum (Fig. 5), it can be seen that in high resolution TEM figure
In (Fig. 4-5), core shell structure is presented in difunctional magnetic fluorescence probe, and using the magnetic microsphere of black as core, the quantum dot of grey is
Shell, and dispersiveness is preferably, grain size distribution is homogeneous, and particle size is about 0.7 μm, and the part that circle circle is lived in addition can see
The tiny oblique line of one rule, illustrating the surface of magnetic microsphere has obvious and uniform lattice, it was demonstrated that quantum dot successfully adsorbs
On magnetic microsphere, and from electron scattering energy spectrum diagram (Fig. 6), it can be found that having ferro element, sulphur on difunctional magnetic fluorescence probe
Element, cadmium element and tellurium element, further demonstrating quantum dot, successfully absorption on magnetic microsphere, successfully synthesizes difunctional
Magnetic fluorescence probe.
2nd, the application of difunctional magnetic fluorescence probe
(1) experiment measure cadmium ion
300 μ L difunctional magnetic fluorescence probe, 600 μ L pH=8.5 are sequentially added in clean quartz colorimetric utensil
Tris-HCl cushioning liquid, 1 μM of EDTA, a series of Cd of concentration is added into cuvette2+, add redistilled water and be settled to
3mL, by XRF fluorescence intensity, detection finds fluorescence intensity change, it is established that the assay method of cadmium ion.Survey
Amount parameter is arranged to：Exciting slit width is 5nm, transmite slit width 5nm, 550~770nm of scanning range, excitation wavelength
395nm。
(2) practical measurement water sample
Take waste water to be used as from North Sea Hepu estuary and Yulin south stream Jiang Suiji and treat test sample.In clean quartz colorimetric utensil
300 μ L difunctional magnetic fluorescence probe, 600 μ L pH=8.5 Tris-HCl cushioning liquid, 1 μM of EDTA is sequentially added,
Testing sample is added into cuvette, redistilled water is added and is settled to 3mL, passes through XRF fluorescence intensity, inspection
Survey and find whether fluorescence intensity changes, realize the measure to cadmium ion.Measurement parameter is arranged to：Exciting slit width is 5nm,
Transmite slit width 5nm, 550~770nm of scanning range, excitation wavelength 395nm.
As shown in Fig. 7 to 10, by the sign (Fig. 7) to cadmium ion detection method, as a is the glimmering of fluorescence probe in Fig. 7
Luminous intensity, c is EDTA and the stronger complexing of cadmium ion in Fig. 7, can be complexed or ban quantum dot on magnetic fluorescent microspheres
The cadmium ion on surface, the defects of destroying quantum dot surface, it result in the reduction of fluorescence intensity；As shown in Figure 8 as EDTA is dense
The continuous increase of degree, the fluorescence of system are constantly quenched；B is cadmium ion when extra cadmium ion is added in system in Fig. 7
The defects of automatically repairing microsphere surface quantum dot, recovers its fluorescence；As shown in figure 9, the continuous increasing with concentration of cadmium ions
Greatly, fluorescence gradually strengthens；Mapped (such as Figure 10) according to the change of concentration of cadmium ions and fluorescence intensity, obtain the work of detection method
Make curve：Y=236551.95X-19644, R 0.9755, sensitivity are 0.5 μM.
Claims (6)
- A kind of 1. difunctional magnetic fluorescence probe preparation method for detecting cadmium ion, it is characterised in that with CdTe/CdS quantum dots and Magnetic fluorescent microspheres with superparamagnetism are material, and it is difunctional to carry out chemical reactive synthesis under the conditions of alkalescence, low temperature, darkness Magnetic fluorescence probe, specifically includes following steps：(1) CdTe/CdS quantum dots are synthesizedUsing one kettle way Hydrothermal Synthesiss CdTe/CdS quantum dots；100mL redistilled waters are added in three-neck flask, add chlorination After cadmium, stirring sequentially adds trisodium citrate, mercaptopropionic acid, is stirred until homogeneous to dissolving；Then, adjusted with sodium hydroxide solution Save pH；Then sodium tellurite, sodium borohydride, stirring to dissolving are separately added into；Finally, magneton is put into, flask is placed in into magnetic force stirs Mix in device, load onto condenser pipe, 90 DEG C of oil bath heatings；During red light quantum point to be obtained, you can take out；Then, CdTe/CdS quantum dot solutions are purified, the quantum dot aqueous solution of synthesis is cooled to room temperature, takes 5-7mL Quantum dot, add the absolute ethyl alcohol of 2 times of volumes, centrifuged using supercentrifuge, remove supernatant after centrifugation, lower sediment is used 5-7mL redistilled water dissolving, it is standby；(2) difunctional magnetic fluorescence probe is synthesizedWeigh that 2mg EDC is soluble in water, add in the quantum dot purification liquid obtained by step (1), stir, to it after dissolving Activated, adjust pH with hydrochloric acid solution, then stir 30min, it is standby；Take 100 μ L, 5mg/mL magnetic fluorescent microspheres to be placed in 10mL PE pipes, add distilled water diluting to 5-7mL, ultrasonic wave to disperse Afterwards, magnetic fluorescent microspheres are mixed with the solution of above-mentioned gained, stirred, then adjust pH with sodium hydroxide solution, finally Add magneton to be placed on magnetic stirring apparatus, sample is reacted in 4 DEG C of dark condition；After reaction terminates, it is centrifuged repeatedly, removes Unreacted quantum dot in supernatant, until the fluorescence of supernatant no longer reduces, obtained magnetic fluorescence probe is dissolved in In distilled water, difunctional magnetic fluorescence probe is produced.
- 2. the difunctional magnetic fluorescence probe preparation method of detection cadmium ion according to claim 1, it is characterised in that step Suddenly in (1), the quality of caddy is 0.1~0.2g, and trisodium citrate is 0.2~0.3g, and mercaptopropionic acid is 50~70 μ L, uses hydrogen Sodium oxide molybdena adjusts pH to 11, sodium tellurite 0.02g, sodium borohydride 0.1g；Centrifuge speed reaches 5000r/ during centrifugation min。
- 3. the difunctional magnetic fluorescence probe preparation method of detection cadmium ion according to claim 1, it is characterised in that step Suddenly hydrochloric acid conditioning solution pH to 6 is used in (2), it is anti-in 4 DEG C of dark environment with sodium hydrate regulator solution pH to 8~9, sample Answer 12 hours.
- 4. the difunctional magnetic fluorescence probe preparation method of detection cadmium ion according to claim 1, it is characterised in that step Suddenly the magnetic fluorescent microspheres in (2) are 500nm amino-magnetic microballoons.
- 5. the difunctional magnetic fluorescence probe obtained according to any preparation method of Claims 1-4.
- 6. application of the difunctional magnetic fluorescence probe in cadmium ion is detected according to claim 5.
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