CN101104807A - Method for synthesizing cadmium selenide quantum dots based on amino acid and polypeptide - Google Patents
Method for synthesizing cadmium selenide quantum dots based on amino acid and polypeptide Download PDFInfo
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- CN101104807A CN101104807A CNA200710052691XA CN200710052691A CN101104807A CN 101104807 A CN101104807 A CN 101104807A CN A200710052691X A CNA200710052691X A CN A200710052691XA CN 200710052691 A CN200710052691 A CN 200710052691A CN 101104807 A CN101104807 A CN 101104807A
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Abstract
The invention discloses a method of synthesizing CdSe quantum dots with Amino acid and polypeptide, comprising the following steps: A, preparing cell-free system of selenium-containing amino acid; B, preparing Cd-glutathione; C, synthesizing CdSe quantum dots. The invention is provided with a simple technology and mild reaction conditions. As no organometallic compounds are included in the preparation, the protection from the inert gas is not needed. The production is safe and low in cost, helpful to the industrial synthesis of the nano-particles (including quantum dots).
Description
Technical field
The invention belongs to nano science, microbiology, the synthetic field of material, specifically, the present invention relates to a kind of cadmium selenide (CdSe) quantum dot synthetic method based on amino acid and polypeptide.
Background technology
Quantum dot (Quantum Dots, QDs) because have unique fluorescence nano effect, for example it excites spectrum width and continuous distribution, emission spectrum is narrow and symmetrical, and emission wavelength can be regulated and control by changing particle diameter and composition, fluorescence intensity is strong, bleaching speed is slow, highly sensitive, and receives much attention.At aspects such as luminescent material, photochemical catalysis, photosensor, fluorescent probe marks wide application prospect is arranged.Wherein, the elementary composition quantum dot of IIB family and VIA family, abbreviate II-VI type quantum dot (as CdSe, CdTe etc.) as, owing to have special good visible and near infrared spectrum district fluorescent emission character, be expected to become novel, convenient biomedical fluorescent probe marker and the transmitter that is suitable for of a class.
In II-VI type quantum dot, CdSe uses main flow quantum dot very widely, its synthetic extensive concern that always is subjected to.The preparation method of relevant this class quantum dot is a lot, and different according to employing raw material and technology are summarized and got up to be broadly divided into the inorganic synthetic route of water and metallic compound-element organism route.The inorganic synthetic route of water comprises: microwave-assisted prepares that quantum dot, supersonic method prepare quantum dot, template prepares quantum dot method etc.These methods are simple to operate, quick, but some microwave phenomenons of also very not understood by people such as non-thermal effect, superthermal effect, effect of ultrasound affect the character such as homogeneity of product.Though and the template preparation method can synthesize a series of nanoparticles (as: CdSe) in diversified limitation template, but after synthetic, how to remove template, perhaps particle is effectively separated from model, not influencing character such as particle diameter, shape then is cumbersome problem.
Metallic compound-element organism route then can use organic reagents such as oxidation tri-n-octyl phosphine (TOPO), cetylamine, octadecylene (ODE) and phosphine compound usually, and usually needs high temperature, reaction under high pressure.In its building-up process, need secluding air and water toward contact, strict to synthesis device.Metallic compound-element organism route can prepare high quality, single (± 5%) II-VI of dispersion quantum dot, and quantum yield is about 10%, and by changing synthesis temperature, can control particle diameter (2.4-23nm).But employed test-run a machine often has bio-toxicity, easy contaminate environment and bring infringement, instability, explosive to human body in preparation process, the appointed condition harshness of needs, and the reaction material cost is higher.These have all hindered quantum dot to a certain extent and have prepared the process of suitability for industrialized production and application.
In the above-mentioned the whole bag of tricks,, all there are problems such as product homogeneity, size to a certain extent though that inorganic synthetic route is polluted is less; And adopt metallic compound-element organism synthetic route, though can use CdO, Cd (Ac)
2Prepare high-quality bare quantum spot in mineral compound, but the preparation of common employed core/shell structure quantum dot still to be used Cd (CH basically
3)
2, Zn (CH
3)
2Make raw material Deng organometallic compound, and all need comparatively harsh reaction conditions.In sum, if these methods can be improved, select raw material cheap, stable in properties, preparation core/shell structure quantum dot under comparatively safe, gentle condition is undoubtedly with significant.
Summary of the invention
The objective of the invention is to be to provide a kind of cadmium selenide (CdSe) quantum dot synthetic method based on amino acid and polypeptide, by this method can be effectively, safely, low toxicity ground carries out the synthetic of CdSe quantum dot, its reaction conditions gentleness, cost of material is cheap, and simple to operate, any biology laboratory all can be finished.
To achieve these goals, the present invention utilizes amino acid and polypeptide to carry out the synthetic of CdSe quantum dots.
A kind of cadmium selenide based on amino acid and polypeptide (CdSe) quantum dot synthetic method, its step is 1) contain the preparation of the biomolecules of selenol group; 2) preparation of cadmium-gsh mixture; 3) the synthetic CdSe quantum dot of reaction.Concrete grammar is as follows:
1) contain the preparation of the biomolecules of selenol group: the biomolecules that directly will contain selenol be dissolved in 20 mmoles/liter phosphate buffered saline buffer (pH 8.0) in, or 20 mmoles/liter phosphate buffered saline buffer (pH 8.0) in dithiothreitol (DTT) the selenium in the biomolecules is reduced into the selenol form.
2) preparation of cadmium-gsh mixture: with cadmium ion (Cd
2+) with gsh be 1: 4 mixed by mole concentration.
3) reaction synthesizing CdSe (CdSe) quantum dot: in there-necked flask, be full of nitrogen, be in there-necked flask to mix at 1: 2 in molar ratio with step 1 and the resulting solution of step 2, and suitably temperature be controlled at 80 ℃～90 ℃, stir simultaneously.Can obtain having the CdSe quantum dot of fluorescence through reaction.
A kind of CdSe quantum dots synthetic method based on amino acid and polypeptide, its technical measures are:
Step 1, contain the preparation of the biomolecules of selenol group.Biomolecules is meant the molecule that can participate in viable cell activity and structure formation at Nucleotide, nucleic acid, amino acid, polypeptide and protein, phosphatide etc.Detailed process of the present invention comprises: the phosphate buffered saline buffer that these biomolecules that contain the selenium element are dissolved in (20 mmoles/liter, pH 8.0) in, or in phosphate buffered saline buffer (20 mmoles/liter, pH 8.0), the selenium in the biomolecules is reduced into the selenol form with dithiothreitol (DTT) (buy try in the Shen, Wuhan chemical industry).In specific examples of the present invention; the standard substance of selenocystine (purchase) in sigma company with 20 mmoles of pH=8.0/liter phosphate buffer soln be made into concentration be 0.5 mmole/liter solution; under nitrogen protection with final concentration be 0.8 mmole/liter dithiothreitol (DTT) 50 ℃ the reaction 2 hours so that obtain containing the seleno-cysteine of selenol.
The preparation of step 2, cadmium-gsh mixture: at first with cadmium ion (Cd
2+) with gsh (buy in Beijing magnificent biochemical reagents company limited) be 1: 4 mixed by mole concentration.In specific examples, gsh and final concentration be 2 mmoles/liter Cadmium chloride fine powder (CdCl
2) mixing (C
Cd2+: C
GSH=4: 1), obtain cadmium gsh mixture, use nitrogen to prevent oxidation simultaneously.
Step 3, reaction synthesizing CdSe (CdSe) quantum dot.Being full of nitrogen in there-necked flask, is in there-necked flask to mix at 1: 2 with step 1 and the resulting solution of step 2 in molar ratio, and suitably heating, obtains having the CdSe quantum dot of fluorescence through reaction.In specific examples, hatched 6～12 hours at 80 ℃～90 ℃ through the solution that step 1 and 2 obtains, promptly obtained fluorescigenic CdSe quantum dot.
Adopt method provided by the invention to compare with present employed method, easy, the strong operability of method of the present invention need not high temperature high pressure device, is fit to directly synthesize at biology laboratory.Compare with the inorganic synthetic route of traditional water, method provided by the invention can successfully be synthesized the CdSe quantum dot, and high temperatures, and synthetic quantum dot comparison separate easily obtains, the good uniformity of product.Metallizing thing-element organism route is compared, method provided by the invention can successfully be synthesized the CdSe quantum dot normal pressure, 80～90 ℃, and do not use virose organic reagent (as: TOPO etc.), building-up process and product environmental pollution are little, need not to use synthetic precursor, stable, the difficult blast of building-up process, synthetic with low cost, not harsh to the requirement of equipment.Generally speaking, method provided by the present invention is greatly improved on the basis of in the past quantum dot synthetic method and improves.
Description of drawings
Fig. 1 utilizes the cell-free system of selenium-containing biological molecule to carry out the picture of CdSe quantum dot synthetic reaction system fluorescence.
This solution has xanchromatic fluorescence under ultra violet lamp.
The ultra-violet absorption spectrum of the CdSe quantum dot after Fig. 2 is synthetic
Its ultra-violet absorption spectrum has maximum absorption band at the 400nm place
The fluorescence emission spectrum of the CdSe quantum dot after Fig. 3 is synthetic
Maximum emission wavelength is 520nm
Fig. 4 temperature of reaction and reaction times are to the influence of CdSe quantum dots fluorescence intensity
Embodiment
Embodiment 1:
Below in conjunction with specific embodiment.Further set forth the present invention, should be appreciated that these embodiment only are used to the present invention is described and are not used in restriction the scope of protection of present invention.
1. contain the preparation of the biomolecules of selenol group:
With the standard substance of selenocystine (purchase) in sigma company with 20 mmoles of pH=8.0/rise phosphate buffer soln be made into concentration be 0.5 mmole/liter solution; under nitrogen protection with final concentration be 0.8 mmole/liter dithiothreitol (DTT) (buy in Shen, Wuhan examination chemical industry) 50 ℃ of reactions 2 hours, obtain containing the seleno-cysteine of selenol group.
2. the preparation of cadmium-gsh mixture:
Equally under nitrogen protection, with the stable final concentration of gsh (buy in Beijing magnificent biochemical reagents company limited) be 2 mmoles/liter Cd
2+(C
Cd2+: C
GSH=4: 1).
3. the CdSe quantum dot is synthesized in reaction.
Under nitrogen protection, will hatch 0～12 hour at 80 ℃ or 85 ℃ or 90 ℃ respectively through the solution that step 1 and 2 obtains.Promptly can be observed fluorescigenic CdSe quantum dot is synthesized.
Table 1 has shown the difference between this programme and other CdSe quantum dots synthetic method.This shows that this synthetic schemes is safer, toxicity is lower, it is littler to pollute.
The contrast of table 1 the present invention and other CdSe synthetic methods
| The present invention | Other synthetic schemes | |
| Raw material | Polypeptide, amino acid | topO, cetylamine, ODE etc. |
| Material toxicity | Do not have | Have |
| Reacting precursor | Do not have | Do not have/have |
| Temperature of reaction | 80～90℃ | 300℃ |
| Reaction pressure | Normal pressure | High pressure |
| Explosion hazard | Non-explosive | Explosive |
| Environmental pollution | Do not have/little | Greatly |
| Reacting phase | Water | Water/oil phase |
Claims (1)
1. CdSe quantum dots synthetic method based on amino acid and polypeptide, it comprises the following steps:
A, contain the preparation of the biomolecules of selenol group: the biomolecules that directly will contain selenol is dissolved in the phosphate buffered saline buffer, or with dithiothreitol (DTT) the selenium in the biomolecules is reduced into the selenol form in phosphate buffered saline buffer;
The preparation of B, cadmium one gsh mixture: the mixed that with cadmium ion and gsh is 1: 4 by mole concentration;
C, reaction synthetizing CdSe quantum dots: in there-necked flask, be full of nitrogen, with the solution of steps A and step B gained is in there-necked flask to mix at 1: 2 in molar ratio, temperature is controlled at 80 ℃～90 ℃, stirs, and obtains having the CdSe quantum dot of fluorescence through reaction.
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| CN200710052691XA CN101104807B (en) | 2007-07-11 | 2007-07-11 | Method for synthesizing cadmium selenide quantum dots based on amino acid and polypeptide |
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| CN101104807B CN101104807B (en) | 2010-08-04 |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102562189A (en) * | 2012-03-14 | 2012-07-11 | 思安新能源股份有限公司 | Low-pressure saturated steam recycling equipment |
| CN102911259A (en) * | 2012-09-21 | 2013-02-06 | 常州大学 | Novel polypeptide ligand modifying quantum dots |
| CN108660185A (en) * | 2018-03-09 | 2018-10-16 | 山东师范大学 | A kind of biosensor and preparation method based on golden selenium key |
| CN108906128A (en) * | 2018-06-13 | 2018-11-30 | 西北工业大学 | A kind of composite photocatalyst material preparation method based on microorganism template |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100487074C (en) * | 2005-12-02 | 2009-05-13 | 华中农业大学 | Method for preparing small-particle-size water-soluble cadium selenide quantum dot and its use |
| CN100352886C (en) * | 2005-12-28 | 2007-12-05 | 武汉大学 | Method for preparing CdSe quantum |
-
2007
- 2007-07-11 CN CN200710052691XA patent/CN101104807B/en not_active Expired - Fee Related
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102562189A (en) * | 2012-03-14 | 2012-07-11 | 思安新能源股份有限公司 | Low-pressure saturated steam recycling equipment |
| CN102911259A (en) * | 2012-09-21 | 2013-02-06 | 常州大学 | Novel polypeptide ligand modifying quantum dots |
| CN108660185A (en) * | 2018-03-09 | 2018-10-16 | 山东师范大学 | A kind of biosensor and preparation method based on golden selenium key |
| CN108906128A (en) * | 2018-06-13 | 2018-11-30 | 西北工业大学 | A kind of composite photocatalyst material preparation method based on microorganism template |
| CN108906128B (en) * | 2018-06-13 | 2021-05-07 | 西北工业大学 | Preparation method of composite photocatalytic material based on microbial template |
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| CN101104807B (en) | 2010-08-04 |
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