CN102994092B - Preparation of cysteine surface modified CdTe or CdTe/CdS quantum dot and method for detecting arsenic by using quantum dot - Google Patents
Preparation of cysteine surface modified CdTe or CdTe/CdS quantum dot and method for detecting arsenic by using quantum dot Download PDFInfo
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Abstract
The invention discloses a preparation method of a cysteine surface modified CdTe or CdTe/CdS quantum dot, which comprises the following steps of: under the condition of room temperature, mixing a cadmium-containing compound powder with cysteine, fully stirring and regulating the pH value to obtain a Cd precursor solution; then adding NaBH4 in Te powder, injecting an acid liquor, bringing H2Te gas generated by acidization under the action of a nitrogen flow out and introducing into the Cd precursor solution, heating for reaction and refluxing to obtain a CdTe quantum dot solution, adding Na2S solution in the CdTe quantum dot solution, and standing to obtain the cysteine surface modified CdTe/CdS nuclear shell quantum dot. The quantum dot disclosed by the invention is added in an arsenic ion-containing solution, and is subjected to fluorescent quantitative characterization by using a fluorospectro photometer to obtain a fluorescent response curve, and therefore, the qualitative or quantitative detection of the concentration of trivalent arsenic ions in a solution to be detected can be realized. The preparation method has the advantages of simpleness in operation, high sensitivity, good selectivity and the like.
Description
Technical field
The present invention relates to a kind of preparation of nano material and arsonium ion detect in application, relate in particular to a kind of halfcystine finishing quantum dot preparation method and arsenic detect in application.
Background technology
Arsenic belongs to non-metallic element, is one of necessary trace element of some animal, but in body, the excessive enrichment of arsenic will cause poisoningly, and severe patient is even fatal.Surface water and Arsenic in Drinking Water pollute has become one of chief culprit of serious threat global human health.Related data shows, at present in global range nearly 1.4 hundred million people touched exceed WHO standard (10 ppb) containing arsenic tap water.Therefore, the monitoring of nature arsenic in water body content is more and more received people's concern.
Arsenic occurring in nature with arsenite [As (III)], arsenate [As (V)] and various organoarsenic (as, methylarsenate and cacodylate) etc. form exist.Compared with pentavalent arsenic, trivalent arsenic more easily enters cell, therefore toxicity is also large than pentavalent arsenic.Therefore, develop a kind of simple, quick, sensitive trivalent arsenic [As (III)] detection technique in having become a reality in the urgent need to.
Quantum dot (Quantum Dots, QDs) is a kind of, size nanocrystal 1 nm～20 nm between elementary composition by II-VI family or III-V family.The volume size of quantum dot and composition are strictly being controlled its Absorption and emission spectra feature, therefore can obtain from ultraviolet near infrared range by varying sized and composition in the quantum dot of emission wavelength arbitrarily.Quantum dot also has the structural performances such as particle size is little, specific surface area is large, and these structural performances have caused the generation of quantum size effect and Dielectric confinement effect, and derive thus unique photoelectric property.Therefore, quantum dot all has potential advantage in Application Areass such as biomarker, chemical-biological detection and information storages.
Halfcystine (Cys)-CdTe/CdS core-shell quanta dots, compared with halfcystine-CdTe quantum dot, has higher fluorescence quantum productive rate and optical stability.Simultaneously, hydrothermal method (Zhang H Y is generally taked in the preparation of halfcystine-CdTe/CdS core-shell quanta dots, Sun P, Liu C, et al. L-Cysteine capped CdTe-CdS core-shell quantum dots:preparation, characterization and immuno-labeling of HeLa cells. Luminescence, 2011, 26 (2): 86-92) water-soluble semi Gelucystine-CdTe quantum dot is carried out to involucrum processing, but there is complex steps in this involucrum method, length consuming time, easily cause the defects such as reagent waste, and its method adopting is by NaBH
4the Te solution of reduction is injected directly in Cd precursor solution, so also may introduce the impurity such as boron-containing compound.
In addition, the method for carrying out arsonium ion detection based on fluorescence quantum at present, there is not yet relevant report.
Summary of the invention
The technical problem to be solved in the present invention is to overcome the deficiencies in the prior art, the preparation method of CdTe quantum dot of the halfcystine finishing that a kind of product foreign matter content is few, reaction conditions is gentle, the process time is short, processing condition are controlled, easy to operation and the preparation method of the CdTe/CdS core-shell quanta dots of halfcystine finishing are provided, also corresponding provide a kind of simple to operate, sensitivity is higher, the good CdTe/CdS core-shell quanta dots of selectivity arsonium ion detect in application.
For solving the problems of the technologies described above, the technical scheme that the present invention proposes is a kind of preparation method of CdTe quantum dot of halfcystine finishing, comprises the following steps:
(1) prepare Cd precursor solution: under room temperature condition, will be containing cadmic compound powder and halfcystine according to the mixed in molar ratio of 1 ︰ (0.5～8.0), magnetic agitation is dissolved in the water mixture, pH value is adjusted to 9.0～11.2(preferably to be regulated with the NaOH solution of 1.0 mol/L～4.0 mol/L), obtain Cd precursor solution;
(2) generate H
2te: under nitrogen protection, add NaBH in Te powder
4the aqueous solution, concussion makes it to mix, and reacts to Te powder and all dissolves, and the acid solution of reinjecting is carried out acidifying, under the effect of nitrogen gas stream, the H that acidifying is produced
2te gas is taken out of;
(3) by the H generating in step (2)
2te gas is passed in the Cd precursor solution making in step (1); The mol ratio of controlling Cd, Te, halfcystine in solution is 1 ︰ (0.1～4) ︰ (0.5～8), be heated to 80 ℃～110 ℃, reaction backflow (return time is preferably 20～40 min), after having reacted, stop heating, obtain the CdTe quantum dot solution of halfcystine finishing, then it is for subsequent use to be cooled to room temperature.
The preparation method of the CdTe quantum dot of above-mentioned halfcystine finishing, the described cadmic compound powder that contains is preferably Cd (ClO
4)
2, CdCl
2or CdAc
2powder.
The preparation method of the CdTe quantum dot of above-mentioned halfcystine finishing, described acid solution is preferably sulfuric acid or the phosphoric acid solution of 0.5 mol/L～5.0 mol/L.
As a total technical conceive, the present invention also provides a kind of preparation method of CdTe/CdS core-shell quanta dots of halfcystine finishing, comprise the following steps: at ambient temperature, in the CdTe quantum dot solution of the halfcystine finishing obtaining to above-mentioned preparation method, add the Na of 0.01 mol/L～1.0 mol/L
2s solution, described Te element and described Na
2the mol ratio of S is controlled at 1: (0.2～5), can prepare the CdTe/CdS core-shell quanta dots of the halfcystine finishing of different fluorescent emission wavelength (530nm～620 nm) after leaving standstill.
The preparation method of the CdTe/CdS core-shell quanta dots of above-mentioned halfcystine finishing, the CdTe quantum dot of described halfcystine finishing is preferably fluorescent emission wavelength at the green fluorescence CdTe of 500nm～550nm quantum dot.
Above-mentioned preparation method is mainly by NaBH based on venting method
4the Te powder of reduction draws and passes into the CdTe quantum dot of preparing halfcystine finishing in Cd precursor solution under acidulated condition, then at ambient temperature, further carries out CdS involucrum on the CdTe of halfcystine finishing quantum dot surface.The venting method that the invention described above adopts has been avoided the introducing of boron-containing compound etc., and involucrum method is simple, gentle, cost is low, and the reaction in whole preparation process is controlled, reproducible, safe and reliable.
As a total technical conceive, the present invention also provides a kind of CdTe/CdS core-shell quanta dots based on halfcystine finishing to detect the method for arsonium ion, comprise the following steps: the CdTe/CdS core-shell quanta dots of halfcystine finishing (being particularly preferably the CdTe/CdS core-shell quanta dots that the invention described above preparation method makes) is diluted, add the solution containing different concns trivalent As (III) ion using phosphoric acid buffer as buffer system, mix standing (approximately 10 min) under rear room temperature, then with spectrophotofluorometer, mixed system is carried out to fluorescent quantitation sign, obtain the CdTe/CdS core-shell quanta dots of described halfcystine finishing for the fluorescence response curve of arsonium ion change in concentration, can realize the qualitative detection to trivalent arsenic ionic concn in solution to be measured according to fluorescence response curve, the arsonium ion of fluorescent quenching effect based on to(for) CdTe/CdS core-shell quanta dots, also can realize the detection by quantitative of arsonium ion.The detection method of this arsonium ion is not only simple to operate, and sensitivity is higher, and selectivity is better.
In the method for above-mentioned detection arsonium ion, preferred, described fluorescence response curve is linear change when trivalent arsenic ionic concn is 14 ng/L～70 ng/L in solution to be measured, be limited to 10 ng/L under the detection of described detection by quantitative.
In the method for above-mentioned detection arsonium ion, in described solution to be measured, preferably add have disodium edta (ethylenediaminetetraacetic acid, concentration is 0.01 mol/L～0.5 mol/L) as sequestering agent.In solution to be measured, add EDTA as sequestering agent, there is good freedom from jamming (EDTA does not disturb trivalent arsenic) for As (III), Pb (II), Sr (II), Na (I), Cu (II), Al (III), Li (I), Fe (III), Zn (II), Mg (II), Mn (II), Ag (I), K (I) ion.
In to solution to be measured, trivalent arsenic ionic concn is carried out before qualitative or detection by quantitative, the preferred first polycarbonate membrane filtration with 0.10 μ m～0.22 μ m by solution to be measured.
Compared with prior art, the invention has the advantages that:
1. aspect prepared by quantum dot, based on venting method by NaBH
4the Te powder of reduction draws to pass in Cd precursor solution and prepares CdTe quantum dot under acidulated condition, avoided the introducing of boron compound etc., is convenient to condition control;
2. at room temperature carry out the involucrum of CdS, as mild as a dove, the involucrum time is short for condition, and involucrum is simple to operate rapidly, only needs 1 min just can complete;
3. a need is by controlling CdTe quantum dot and the Na of halfcystine finishing
2the molar ratio of S can obtain the CdTe/CdS core-shell quanta dots of the halfcystine finishing of different emission;
4. the quantum dot size homogeneous that prepared by the present invention, monodispersity is good, and quantum dot nano-particle spectrum is controlled, there is extremely good spectrum property, exciting light spectrum width and continuous, fluorescence spectrum is narrow and symmetrical, photochemical stability is strong, for further applied research is laid a good foundation;
5. the CdTe/CdS core-shell quanta dots that prepared by the present invention is for the detection of arsonium ion, and simple to operate, sensitivity is higher, and selectivity is better.
Accompanying drawing explanation
Fig. 1 is the easy device structural representation of preparing water-soluble semi Gelucystine-CdTe quantum dot in the embodiment of the present invention.
Fig. 2 is water-soluble semi Gelucystine-CdTe quantum dot ultraviolet-visible absorption spectroscopy and corresponding fluorescence emission spectrum thereof in the embodiment of the present invention.
Fig. 3 is the fluorescence emission spectrum of halfcystine-CdTe/CdS core-shell quanta dots of the different emission prepared in the embodiment of the present invention.
Fig. 4 is halfcystine-CdTe/CdS core-shell quanta dots of the different emission prepared in embodiment of the present invention fluorogram of taking pictures under 365 nm purple lights irradiate.
Fig. 5 be in the embodiment of the present invention halfcystine-CdTe/CdS core-shell quanta dots fluorescence intensity for the response curve of arsonium ion concentration.
Embodiment
Below in conjunction with Figure of description, the invention will be further described with concrete preferred embodiment, but protection domain not thereby limiting the invention.
embodiment:
1. the preparation of halfcystine-CdTe quantum dot.
A preparation method for the CdTe quantum dot of halfcystine finishing of the present invention, comprises the following steps:
(1) prepare Cd precursor solution: adopt the easy device shown in Fig. 1 to be prepared, first, under room temperature condition, in 100mL beaker, add successively 0.263g Cd (ClO
4)
26H
2o(CdCl
2or CdAc
2powder also can) and 0.186 g halfcystine (Cd
2+with the mol ratio of halfcystine be 1 ︰ 2.4), then add 20 mL water dissolution, constantly under magnetic agitation, mixture being dissolved in the water, obtain Cd precursor solution; With the NaOH solution of 1 mol/L by the pH value of Cd precursor solution be adjusted to 9.0(9.0～11.2 all can), proceed in the three-necked flask on the left side of easy device shown in Fig. 1 after being settled to 40 mL;
(2) generate H
2te: add 0.03gTe powder, 0.067g NaBH in the three-necked flask on the right in Fig. 1
4with 3 mL ultrapure waters, under magnetic agitation effect, logical N
2deoxygenation 30 min, Te dissolves gradually, and solution slowly reddens, and reacts to Te powder and all dissolves, final pulverize redness; Under nitrogen protection, in the solution after dissolving to Te powder with syringe, dropwise drip the H of 10 mL 4 mol/L
2sO
4solution carries out acidifying, continues logical nitrogen, under the effect of nitrogen gas stream, and the H that acidifying is generated
2te gas slowly enters into the Cd precursor solution of left side three-necked flask with nitrogen gas stream;
(3) by the H generating in above-mentioned steps (2)
2te gas is passed in the Cd precursor solution making in step (1); Control Cd in reaction soln
2+, Te
2+, halfcystine mol ratio be 1 ︰ 0.5 ︰ 2.4, be heated to 80 ℃, the about 40min of reaction backflow, when reacted mixing solutions is under ultra violet lamp when transmitting green fluorescence, can stop refluxing and heating, obtain the CdTe quantum dot solution (fluorescent emission wavelength is greatly about 500～550 nm) of the halfcystine finishing of green fluorescence.
Adopt the CdTe quantum dot solution of the halfcystine finishing of ultraviolet-visible pectrophotometer to above-mentioned preparation to carry out absorption spectrometry.Simultaneously, adopt spectrophotofluorometer to carry out fluorescence emission spectrum mensuration to the CdTe quantum dot solution of halfcystine finishing, photomultiplier transit tube voltage is set to 700 V, and excitation wavelength is 370 nm, excite and launch slit width to be 5nm, detected result as shown in Figure 2.Fluorescent emission peak position wavelength is 544nm, occurs the first absorption peak at 505nm place.
the preparation of halfcystine-CdTe/CdS core-shell quanta dots.
A preparation method for the CdTe/CdS core-shell quanta dots of halfcystine finishing of the present invention, comprises the following steps:
The CdTe quantum dot solution of halfcystine finishing of preparation in above-mentioned steps 1 is cooled to room temperature, and the insolubles of not participating in reaction be sunken to completely bottle at the bottom of after, get upper strata liquid; In the CdTe quantum dot mother liquor of the halfcystine finishing obtaining to above-mentioned preparation method at ambient temperature,, add different volumes 0.02 mol/L Na
2s solution, constantly fully mixes at normal temperatures the CdTe quantum dot solution of halfcystine finishing and sodium sulfide solution under agitation condition, and makes Te and Na with different mol ratios
2the mol ratio of S is controlled at respectively 1: 0,1: 0.768,1: 1.150,1:1.536,1:1.920,1:2.304,1:2.688,1:3.072, leave standstill the CdTe/CdS core-shell quanta dots that can prepare fluorescent emission wavelength after 1 min and be respectively the halfcystine finishing of 544 nm, 550 nm, 570 nm, 578 nm, 599 nm, 609 nm, 614 nm, 615 nm, after centrifugal, obtain the CdTe/CdS core-shell quanta dots of the halfcystine finishing of purifying, and put into 4 ℃ of refrigerators and preserve.
in actual sample water sample, carry out arsenic based on halfcystine-CdTe/CdS core-shell quanta dots and detect application.
By after the CdTe/CdS core-shell quanta dots dilute with water of the halfcystine finishing of preparation in above-mentioned steps 2, adopt ultraviolet-visible pectrophotometer to carry out absorption spectrometry to the CdTe/CdS core-shell quanta dots of prepared halfcystine finishing.Meanwhile, adopt spectrophotofluorometer to carry out fluorescence emission spectrum mensuration to the CdTe/CdS core-shell quanta dots of halfcystine finishing, photomultiplier transit tube voltage is set to 700 V, and excitation wavelength is 370 nm, excites and launch slit width to be 5 nm.
Fig. 3 is water-soluble semi Gelucystine-CdTe quantum dot and the Na of above-mentioned different mol ratio example
2the fluorescence emission spectrum of S CdTe/CdS core-shell quanta dots of prepared halfcystine finishing after mixing.Spectroscopic data is as shown in Figure 3 visible, and gained quantum dot absorption spectrum is wider and continuous, and emission wavelength is narrow and symmetrical, has very good spectrum property.
Fig. 4 is water-soluble semi Gelucystine-CdTe quantum dot and the Na of above-mentioned different mol ratio example
2the take pictures fluorogram of the CdTe/CdS core-shell quanta dots of S prepared halfcystine finishing after mixing under 365 nm purple lights irradiate, wherein from left to right, the color of CdTe/CdS core-shell quanta dots presents dark green, green, light green, orange, pale red, red, dark red variation successively.
A kind of CdTe/CdS core-shell quanta dots based on halfcystine finishing of the present invention detects the method for arsonium ion, comprise the following steps: after by the fluorescent emission peak position wavelength of above-mentioned preparation being the CdTe/CdS core-shell quanta dots dilution of halfcystine finishing of 578 nm, add the solution containing different concns trivalent As (III) ion using phosphoric acid buffer as buffer system, mix standing 10 min under rear room temperature, then with spectrophotofluorometer, mixed system is carried out to fluorescent quantitation sign, obtain the CdTe/CdS core-shell quanta dots of halfcystine finishing for the fluorescence response curve (referring to Fig. 5) of arsonium ion change in concentration, can realize the qualitative or detection by quantitative to trivalent arsenic ionic concn in solution to be measured according to fluorescence response curve.
Another employing Hunan Xiang River water is that actual water sample detects, and adopts standard addition method to measure (referring to table 1).First utilizing pore size is that the polycarbonate membrane of 0.22 μ m removes by filter insoluble substance in actual water sample.Sample is carried out to fluoroscopic examination as fluorescence background.Then in diluted actual water sample, add 0.05 mol/L EDTA to carry out ion and shelter, add respectively the trivalent arsenic ion of 14 ng/L, 28 ng/L, 42 ng/L, 70 ng/L simultaneously.After by fluorescent emission peak position wavelength being the CdTe/CdS core-shell quanta dots dilution of halfcystine finishing of 578 nm, add the solution containing different concns trivalent As (III) ion using phosphoric acid buffer as buffer system, mix standing 10 min under rear room temperature, then with spectrophotofluorometer, mixed system is carried out to fluorometric assay, parallel sample is measured three times.Can obtain the measurement result of trivalent arsenic ionic concn according to the fluorescence response typical curve shown in Fig. 5, further can be recycled rate (seeing table 1).
Table 1: in the present embodiment, halfcystine-CdTe/CdS core-shell quanta dots detects the determination of recovery rates result of As (III).
| Add value (ng/L) | Measured value (ng/L) | The rate of recovery (%) |
| 14.0 | 13.5 ± 0.2 | 96.5 ± 1.5 |
| 28.0 | 29.4 ± 0.3 | 105.0 ± 1.3 |
| 42.0 | 43.3 ± 0.2 | 103.2 ± 0.5 |
| 70.0 | 70.7 ± 0.1 | 101.1 ± 0.2 |
From upper table 1, the detection effect of trivalent arsenic ionic concn is better.
Claims (5)
1. a preparation method for the CdTe/CdS core-shell quanta dots of halfcystine finishing, is characterized in that, comprises the following steps: at ambient temperature, and to the Na that adds 0.01mol/L～1.0mol/L in the CdTe quantum dot solution of halfcystine finishing
2s solution, described Te and described Na
2the mol ratio of S is controlled at 1: (0.2～5), can prepare the CdTe/CdS core-shell quanta dots of the halfcystine finishing of different fluorescent emission wavelength after leaving standstill; The preparation method of the CdTe quantum dot of described halfcystine finishing, comprises the following steps:
(1) prepare Cd precursor solution: under room temperature condition, will be containing cadmic compound powder and halfcystine according to 1: the mixed in molar ratio of (0.5～8.0), fully stir mixture is dissolved in the water, pH value is adjusted to 9.0～11.2, obtain Cd precursor solution;
(2) generate H
2te: under nitrogen protection, add NaBH in Te powder
4the aqueous solution, concussion makes it to mix, and reacts to Te powder and all dissolves, and the acid solution of reinjecting is carried out acidifying, under the effect of nitrogen gas stream, the H that acidifying is produced
2te gas is taken out of;
(3) by the H generating in step (2)
2te gas is passed in the Cd precursor solution making in step (1); The mol ratio of controlling Cd, Te, halfcystine in solution is 1: (0.1～4): (0.5～8), being heated to 80 ℃～110 ℃, reaction refluxes, and stops heating after having reacted, and obtains the CdTe quantum dot solution of halfcystine finishing.
2. the preparation method of the CdTe/CdS core-shell quanta dots of halfcystine finishing according to claim 1, is characterized in that: described is Cd (ClO containing cadmic compound powder
4)
2, CdCl
2or CdAc
2powder.
3. the preparation method of the CdTe/CdS core-shell quanta dots of halfcystine finishing according to claim 1 and 2, is characterized in that: the sulfuric acid that described acid solution is 0.5mol/L～5.0mol/L or phosphoric acid solution.
4. the preparation method of the CdTe/CdS core-shell quanta dots of halfcystine finishing according to claim 1 and 2, is characterized in that: in described step (1), carry out pH value regulate with the NaOH solution of 1.0mol/L～4.0mol/L.
5. the preparation method of the CdTe/CdS core-shell quanta dots of halfcystine finishing according to claim 1, is characterized in that: the CdTe quantum dot of described halfcystine finishing is that fluorescent emission wavelength is at the green fluorescence CdTe of 500nm～550nm quantum dot.
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| CN104650856B (en) * | 2015-02-26 | 2017-01-04 | 江汉大学 | A kind of preparation method of cadmiumsulfide quantum dot solution |
| CN104789208A (en) * | 2015-04-09 | 2015-07-22 | 天津师范大学 | Preparation method and application of CD-PEI (carbon dot-polyethyleneimine) |
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| CN105954248B (en) * | 2016-05-20 | 2018-10-26 | 南昌大学 | Arsenite detection method based on DNA biology quantum dot enhancement effect of fluorescences |
| CN111359630A (en) * | 2018-12-25 | 2020-07-03 | Tcl集团股份有限公司 | Composite material and preparation method thereof |
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