CN105400517A - Method for preparing dual-functional magnetic fluorescent probe for detecting cadmium ions and application thereof - Google Patents
Method for preparing dual-functional magnetic fluorescent probe for detecting cadmium ions and application thereof Download PDFInfo
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- CN105400517A CN105400517A CN201510728313.3A CN201510728313A CN105400517A CN 105400517 A CN105400517 A CN 105400517A CN 201510728313 A CN201510728313 A CN 201510728313A CN 105400517 A CN105400517 A CN 105400517A
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- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
- C09K11/88—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing selenium, tellurium or unspecified chalcogen elements
- C09K11/881—Chalcogenides
- C09K11/883—Chalcogenides with zinc or cadmium
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- C—CHEMISTRY; METALLURGY
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
- G01N21/64—Fluorescence; Phosphorescence
- G01N21/6428—Measuring fluorescence of fluorescent products of reactions or of fluorochrome labelled reactive substances, e.g. measuring quenching effects, using measuring "optrodes"
- G01N21/643—Measuring fluorescence of fluorescent products of reactions or of fluorochrome labelled reactive substances, e.g. measuring quenching effects, using measuring "optrodes" non-biological material
Abstract
The invention discloses a dual-functional magnetic fluorescent probe for detecting cadmium ions and a preparation method thereof. According to the method, CdTe/CdS quantum dots and magnetic fluorescent microspheres with superparamagnetism serving as materials are subjected to chemical reactions under alkaline, low-temperature and dark conditions to synthesize the dual-functional magnetic fluorescent probe. The preparation method is quick, simple and convenient, and has good sensitivity; and the synthesized dual-functional magnetic fluorescent probe has the characteristics of controllable grain diameter, high fluorescent strength, good dispersion and magnetic separation of magnetic microspheres, and can be reclaimed and recycled. The dual-functional magnetic fluorescent probe can be used for detecting heavy metal cadmium ions with advantages of quickness, convenience and sensitivity, and the dual-functional magnetic fluorescent probe is suitable for market popularization and application.
Description
Technical field
The invention belongs to detection of heavy metal ion field, particularly relate to a kind of difunctional magnetic fluorescence probe preparation method and the application thereof that detect cadmium ion.
Background technology
Developing rapidly of the modernization of industry and constantly bringing forth new ideas of Chemical Engineering Technology, cadmium is widely used in Chemical Manufacture, but constantly increases along with cadmium usage quantity, and the pollution that cadmium causes starts the attention causing people.Cadmium ion is one of source of pollution the most serious in heavy metal contamination, its toxicity hazard produced is much larger than other metallic pollutions, it not only cannot degrade by organism on the earth, and by other chemical actions such as enrichments, can indirectly or directly threaten to the health of the Nature biology and the mankind.The traditional detection method of heavy metal ion is varied, in environment measuring, the method detecting cadmium ion mainly contains: electrochemical methods, graphite oven atomic absorption, ultraviolet spectrophotometry, anodic stripping voltammetry, atomic absorption spectrometry, inductively coupled plasma mass spectrometry etc., though these methods can carry out certain analysis and determination to cadmium ion, also cadmium ion content can be measured to some extent, but their most complicated operations, sample preparation bothers, need large-scale instrument, analysis cost is high, analysis time is long, and interfering ion more time, error is large, have a strong impact on the accuracy of measurement result, some detecting step is loaded down with trivial details simultaneously, be not suitable for analysis and the detection of site environment, be difficult to apply.
Semiconductor-quantum-point is because of its excellent performance, and become star's material of nearest material science, it is wider that it has excitation wavelength range, continuously, emission peak is narrower, and is symmetric in distribution, mutual overlap is less, be not easy mutual interference, productive rate is higher, good light stability, anti-light whitening capacity is strong, and fluorescence lifetime is long, there is the advantages such as good spatial compatibility, present wide application prospect in ion measurement, bioprobe, cell marking and the field such as imaging, drug determination.
Fluorescent microsphere refers to diameter at nano level in micro-scaled range, and load has fluorescent substance, stimulates the solia particle that can inspire fluorescence by outside energy.Its profile can be arbitrary shape, and representative configuration is spherical.The study hotspot of current detection of heavy metal ion is the sensitivity of raising biological detection and is amplified by detection signal, and fluorescent microsphere is as a kind of fluorescent material that is novel, that have special optical, electrical, magnetic property, is also widely used in the aspects such as bio-imaging, biological detection and ion measurement.
Summary of the invention
The technical problem to be solved in the present invention is to provide difunctional magnetic fluorescence probe preparation method and the application thereof of a kind of technics comparing detection cadmium ion simple, convenient to operation, gained difunctional magnetic fluorescence probe pin fluorescence intensity is high, good dispersity and have the feature of magnetic microsphere magnetic resolution, can be recycled.
For solving the problems of the technologies described above, the present invention is by the following technical solutions: the difunctional magnetic fluorescence probe preparation method detecting cadmium ion, with CdTe/CdS quantum dot and there is the magnetic fluorescent microspheres of superparamagnetism for material, under alkalescence, low temperature, dark condition, carry out the difunctional magnetic fluorescence probe of chemical reactive synthesis.
The difunctional magnetic fluorescence probe preparation method of above-mentioned detection cadmium ion, comprises the following steps:
(1) CdTe/CdS quantum dot is synthesized
Adopt one kettle way Hydrothermal Synthesis CdTe/CdS quantum dot; In three-necked flask, add 100mL redistilled water, after adding Cadmium chloride fine powder, be stirred to dissolving, add trisodium citrate, thiohydracrylic acid successively, be stirred to evenly; Then, pH is regulated with sodium hydroxide solution; Then add sodium tellurite, sodium borohydride respectively, be stirred to dissolving; Finally, put into magneton, flask is placed in magnetic stirring apparatus, load onto prolong, 90 DEG C of oil bath heating; During red light quantum point to be obtained, can take out;
Then, CdTe/CdS quantum dot solution is purified, the quantum dot aqueous solution of synthesis is cooled to room temperature, get the quantum dot of 5-7mL, add the dehydrated alcohol of 2 times of volumes, use supercentrifuge centrifugal, supernatant liquor is removed, the second distillation water dissolution of lower sediment 5-7mL after centrifugal, for subsequent use;
(2) difunctional magnetic fluorescence probe is synthesized
The EDC taking 2mg is soluble in water, adds in the quantum dot purification liquid of step (1) gained, stir, activate it, regulate pH with hydrochloric acid soln, then stir 30min after dissolving, for subsequent use;
Get 100 μ L, 5mg/ml magnetic fluorescent microspheres is placed in the PE pipe of 10ml, adding distil water is diluted to 5-7ml, after ultrasonic wave dispersion, the solution of magnetic fluorescent microspheres with above-mentioned gained is mixed, stirs, then regulate pH with sodium hydroxide solution, finally adding magneton is placed on magnetic stirring apparatus, and sample is reacted in the dark condition of 4 DEG C; After reaction terminates, repeatedly centrifugal, remove unreacted quantum dot in supernatant liquor, until the fluorescence of supernatant liquor no longer reduces, the magnetic fluorescence probe obtained is dissolved in distilled water, obtains difunctional magnetic fluorescence probe.
In step (1), the quality of Cadmium chloride fine powder is 0.1 ~ 0.2g, and trisodium citrate is 0.2 ~ 0.3g, and thiohydracrylic acid is 50 ~ 70 μ L, and regulate pH to 11 with sodium hydroxide, sodium tellurite is 0.02g, and sodium borohydride is 0.1g; Time centrifugal, centrifuge speed reaches 5000r/min.
With hydrochloric acid conditioning solution pH to 6 in step (2), with sodium hydrate regulator solution pH to 8 ~ 9, sample reacts 12 hours in the dark environment of 4 DEG C.
Magnetic fluorescent microspheres in step (2) is 500nm amino-magnetic microballoon.
The difunctional magnetic fluorescence probe that above-mentioned preparation method obtains.
Above-mentioned difunctional magnetic fluorescence probe is detecting the application in cadmium ion.
For traditional heavy metal cadmium ion detection exist expensive, operate complicated, that the time is tediously long problem, there is based on magnetic microsphere the feature of good fluorescence character, inventor has devised a kind of difunctional magnetic fluorescence probe detecting cadmium ion and preparation method thereof, this method is with CdTe/CdS quantum dot and have the magnetic fluorescent microspheres of superparamagnetism for material, carries out the difunctional magnetic fluorescence probe of chemical reactive synthesis under alkalescence, low temperature, dark condition.Preparation method of the present invention is quick, easy, susceptibility is good, and the difunctional magnetic fluorescence probe size tunable of synthesis, fluorescence intensity are high, good dispersity, have the feature of magnetic microsphere magnetic resolution, can recycle, can be recycled.Apply the detection that difunctional magnetic fluorescence probe of the present invention carries out heavy metal cadmium ion, there is quick, easy, sensitive advantage, be applicable to marketing application.
Accompanying drawing explanation
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 is difunctional magnetic fluorescence probe image on (right side) under (left side) and ultraviolet lamp under white light.
Fig. 4 is the Electronic Speculum figure 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 spectrogram.
Fig. 7 is cadmium ion detection method phenogram.
Fig. 8 is that different EDTA concentration is to the effect diagram of system fluorescence.
Fig. 9 is the variation diagram of concentration of cadmium ions and fluorescence intensity.
Figure 10 is the working curve that cadmium ion measures.
Embodiment
One, the preparation of difunctional magnetic fluorescence probe
With CdTe/CdS quantum dot and there is the magnetic fluorescent microspheres of superparamagnetism for material, under alkalescence, low temperature, dark condition, carry out chemical reactive synthesis, specifically comprise the following steps:
(1) CdTe/CdS quantum dot is synthesized
Adopt one kettle way Hydrothermal Synthesis CdTe/CdS quantum dot; In three-necked flask, add 100mL redistilled water, after adding Cadmium chloride fine powder 0.1 ~ 0.2g, be stirred to dissolving, add trisodium citrate 0.2 ~ 0.3g, thiohydracrylic acid (MPA) 50 ~ 70 μ L successively, be stirred to evenly; Then, regulate about pH to 11 then to add sodium tellurite 0.02g, sodium borohydride 0.1g respectively with the sodium hydroxide solution of existing preparation, be stirred to dissolving; Finally, put into magneton, flask is placed in magnetic stirring apparatus, load onto prolong, 90 DEG C of oil bath heating; During red light quantum point to be obtained, can take out;
Then, CdTe/CdS quantum dot solution is purified, the quantum dot aqueous solution of synthesis is cooled to room temperature, get the quantum dot of 5-7mL, add the dehydrated alcohol of 2 times of volumes, use supercentrifuge centrifugal (5000r/min), after centrifugal, remove supernatant liquor, the second distillation water dissolution of lower sediment 5-7mL, for subsequent use;
(2) difunctional magnetic fluorescence probe is synthesized
The EDC taking 2mg is soluble in water, adds in the quantum dot purification liquid of step (1) gained, stir, activate it after dissolving, regulates about pH to 6, then stir 30min with hydrochloric acid soln, for subsequent use;
Get 100 μ L, 5mg/ml magnetic fluorescent microspheres is placed in the PE pipe of 10ml, adding distil water is diluted to 5-7ml, after ultrasonic wave dispersion, the solution of magnetic fluorescent microspheres with above-mentioned gained is mixed, stirs, then regulate pH to 8 ~ 9 with sodium hydroxide solution, finally adding magneton is placed on magnetic stirring apparatus, and sample is reacted 12 hours in the dark condition of 4 DEG C; After reaction terminates, repeatedly centrifugal, remove unreacted quantum dot in supernatant liquor, until the fluorescence of supernatant liquor no longer reduces, the magnetic fluorescence probe obtained is dissolved in distilled water, obtains difunctional magnetic fluorescence probe.
As shown in Figures 1 to 6, carry out ultra-violet absorption spectrum (Fig. 1), fluorescence spectrum (Fig. 2) and under white light and ultraviolet lamp, contrast (Fig. 3) characterizing by the difunctional magnetic fluorescence probe of preparation, can prove that quantum dot is successfully adsorbed on magnetic microsphere, there is stronger fluorescence intensity, can magnetic resolution, and in the process of synthesizing magnetic fluorescent probe, quantum dot is not reunited, better dispersed.
By Electronic Speculum (Fig. 4, Fig. 5) characterize with electron scattering power spectrum (Fig. 5), can see in high resolution TEM figure (Fig. 4-5), difunctional magnetic fluorescence probe presents nucleocapsid structure, with the magnetic microsphere of black for core, the quantum dot of grey is shell, and it is better dispersed, grain size distribution is homogeneous, size is about 0.7 μm, in addition the part that circle circle is lived can see the oblique line that a rule is tiny, illustrate that the surface of magnetic microsphere has obviously and uniform lattice, demonstrate quantum dot to be successfully adsorbed on magnetic microsphere, and from electron scattering energy spectrogram (Fig. 6), can find that difunctional magnetic fluorescence probe has ferro element, element sulphur, cadmium element and tellurium element, further demonstrate quantum dot to be successfully adsorbed on magnetic microsphere, successfully synthesize difunctional magnetic fluorescence probe.
Two, the application of difunctional magnetic fluorescence probe
(1) test determination cadmium ion
In clean quartz colorimetric utensil, add the difunctional magnetic fluorescence probe of 300 μ L, the Tris-HCl buffered soln of 600 μ LpH=8.5, the EDTA of 1 μM successively, in cuvette, add the Cd of a series of concentration
2+, add redistilled water and be settled to 3mL, by fluorescence spectrophotometer fluorescence intensity, detect and find fluorescence intensity change, set up the measuring method of cadmium ion.Measuring parameter is set to: excite slit width to be 5nm, launches slit width 5nm, sweep limit 550 ~ 770nm, excitation wavelength 395nm.
(2) practical measurement water sample
Waste water is got as treating test sample from Hepu, North Sea estuario and Yulin south stream Jiang Suiji.The difunctional magnetic fluorescence probe of 300 μ L, the Tris-HCl buffered soln of 600 μ LpH=8.5, the EDTA of 1 μM is added successively in clean quartz colorimetric utensil, testing sample is added in cuvette, add redistilled water and be settled to 3mL, by fluorescence spectrophotometer fluorescence intensity, detect and find whether fluorescence intensity changes, and realizes the mensuration to cadmium ion.Measuring parameter is set to: excite slit width to be 5nm, launches slit width 5nm, sweep limit 550 ~ 770nm, excitation wavelength 395nm.
As shown in Fig. 7 to 10, by the sign (Fig. 7) to cadmium ion detection method, as the fluorescence intensity that a in Fig. 7 is fluorescent probe, in Fig. 7, c is the complexing action that EDTA and cadmium ion are stronger, can complexing or ban the cadmium ion of quantum dot surface on magnetic fluorescent microspheres, destroy the defect of quantum dot surface, result in the reduction of fluorescence intensity; As shown in Figure 8 along with the continuous increase of EDTA concentration, the continuous quencher of fluorescence of system; In Fig. 7, b is that cadmium ion automatically repairs the defect of microsphere surface quantum dot, and its fluorescence is recovered in time adding extra cadmium ion in system; As shown in Figure 9, along with the continuous increase of concentration of cadmium ions, fluorescence strengthens gradually; Change according to concentration of cadmium ions and fluorescence intensity is mapped (as Figure 10), obtains the working curve of detection method: Y=236551.95X-19644, R are 0.9755, and sensitivity is 0.5 μM.
Claims (7)
1. one kind is detected the difunctional magnetic fluorescence probe preparation method of cadmium ion, it is characterized in that with CdTe/CdS quantum dot and there is the magnetic fluorescent microspheres of superparamagnetism for material, under alkalescence, low temperature, dark condition, carrying out the difunctional magnetic fluorescence probe of chemical reactive synthesis.
2. the difunctional magnetic fluorescence probe preparation method of detection cadmium ion according to claim 1, is characterized in that comprising the following steps:
(1) CdTe/CdS quantum dot is synthesized
Adopt one kettle way Hydrothermal Synthesis CdTe/CdS quantum dot; In three-necked flask, add 100mL redistilled water, after adding Cadmium chloride fine powder, be stirred to dissolving, add trisodium citrate, thiohydracrylic acid successively, be stirred to evenly; Then, pH is regulated with sodium hydroxide solution; Then add sodium tellurite, sodium borohydride respectively, be stirred to dissolving; Finally, put into magneton, flask is placed in magnetic stirring apparatus, load onto prolong, 90 DEG C of oil bath heating; During red light quantum point to be obtained, can take out;
Then, CdTe/CdS quantum dot solution is purified, the quantum dot aqueous solution of synthesis is cooled to room temperature, get the quantum dot of 5-7mL, add the dehydrated alcohol of 2 times of volumes, use supercentrifuge centrifugal, supernatant liquor is removed, the second distillation water dissolution of lower sediment 5-7mL after centrifugal, for subsequent use;
(2) difunctional magnetic fluorescence probe is synthesized
The EDC taking 2mg is soluble in water, adds in the quantum dot purification liquid of step (1) gained, stir, activate it, regulate pH with hydrochloric acid soln, then stir 30min after dissolving, for subsequent use;
Get 100 μ L, 5mg/ml magnetic fluorescent microspheres is placed in the PE pipe of 10ml, adding distil water is diluted to 5-7ml, after ultrasonic wave dispersion, the solution of magnetic fluorescent microspheres with above-mentioned gained is mixed, stirs, then regulate pH with sodium hydroxide solution, finally adding magneton is placed on magnetic stirring apparatus, and sample is reacted in the dark condition of 4 DEG C; After reaction terminates, repeatedly centrifugal, remove unreacted quantum dot in supernatant liquor, until the fluorescence of supernatant liquor no longer reduces, the magnetic fluorescence probe obtained is dissolved in distilled water, obtains difunctional magnetic fluorescence probe.
3. the difunctional magnetic fluorescence probe preparation method of detection cadmium ion according to claim 1, it is characterized in that in step (1), the quality of Cadmium chloride fine powder is 0.1 ~ 0.2g, trisodium citrate is 0.2 ~ 0.3g, thiohydracrylic acid is 50 ~ 70 μ L, regulate pH to 11 with sodium hydroxide, sodium tellurite is 0.02g, and sodium borohydride is 0.1g; Time centrifugal, centrifuge speed reaches 5000r/min.
4. the difunctional magnetic fluorescence probe preparation method of detection cadmium ion according to claim 1, it is characterized in that in step (2) with hydrochloric acid conditioning solution pH to 6, with sodium hydrate regulator solution pH to 8 ~ 9, sample reacts 12 hours in the dark environment of 4 DEG C.
5. the difunctional magnetic fluorescence probe preparation method of detection cadmium ion according to claim 1, is characterized in that the magnetic fluorescent microspheres in step (2) is 500nm amino-magnetic microballoon.
6. according to the difunctional magnetic fluorescence probe that the arbitrary described preparation method of claim 1 to 5 obtains.
7. difunctional magnetic fluorescence probe is detecting the application in cadmium ion according to claim 6.
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| CN112500847A (en) * | 2020-11-16 | 2021-03-16 | 武汉理工大学 | Cadmium ion probe based on quantum dot fluorescence resonance energy transfer system and preparation method thereof |
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| CN112500847A (en) * | 2020-11-16 | 2021-03-16 | 武汉理工大学 | Cadmium ion probe based on quantum dot fluorescence resonance energy transfer system and preparation method thereof |
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