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Amphiphilic macromolecular modified oil-soluble nuclear/shell quantum dots and preparation method

A polymer and amphiphilic technology, which is applied in the field of nanomaterial preparation and biochemical multi-throughput detection, can solve the problems of non-specific bonding, low yield, and damage to the surface structure of quantum dots, so as to reduce toxicity, simple preparation method, The effect of stable fluorescence properties

Active Publication Date: 2012-11-07
南通药享科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] At present, there are many literature reports on the hydrophilic modification of quantum dots, such as patent CN101104806, which uses hydrophilic silicate to coat quantum dots, but the reaction conditions are not easy to control, the reproducibility is poor, and the yield is low. In the later application, non-specific adsorption Serious; patent CN101250403 uses long-chain mercapto compounds to coat quantum dots, but the combination of mercaptocarboxylic acid and quantum dots is not stable, and under the condition of a physiological solution with a pH of 7-8.5, the carboxyl groups on the surface of quantum dots will dissociate and cause Severe non-specific bonding; patents CN1712489 and CN101012373A both use core / shell quantum dots for hydrophilic modification, but the difference in lattice parameters between the core and shell affects the crystal structure and fluorescence efficiency of quantum dots, and The polymer used may destroy the surface structure of quantum dots and affect the uniformity of the surface of quantum dots

Method used

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  • Amphiphilic macromolecular modified oil-soluble nuclear/shell quantum dots and preparation method
  • Amphiphilic macromolecular modified oil-soluble nuclear/shell quantum dots and preparation method
  • Amphiphilic macromolecular modified oil-soluble nuclear/shell quantum dots and preparation method

Examples

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Effect test

Embodiment 1

[0027] (1) Take 1 mL of chloroform solution of CdSe nuclear quantum dots, add 3 mL of octadecene, and take 0.1 g of octadecylamine and tri-n-octyl phosphorus oxide in a flask; after 30 minutes of argon gas, heat to 100 ° C, After keeping for 8 minutes, continue to heat up to 200°C; calculate the Cd required to prepare each layer of quantum dots 2+ , Zn 2+ , S 2- The amount, dropwise added the special Cd, Zn, S shell precursor solution; prepared CdSe / CdS / Cd 0.4 Zn 0.6 S / ZnS quantum dots were centrifuged and purified twice with acetone, and then stored in a sealed, dark place at low temperature.

[0028] (2) Poly-tert-butylacrylic acid, hexylamine and coupling agent EDC.HCl are mixed and dissolved in dimethylformamide, wherein the molar ratio of poly-tert-butylacrylic acid to hexylamine is 1:20, coupling agent and hexylamine The molar ratio was 1:1, and the reaction was carried out for 8 hours to obtain poly-tert-butylacrylic acid-hexylamine whose long chain was polyacrylic ...

Embodiment 2

[0033] (1) Take 1.75mL of CdSe nuclear quantum dot chloroform solution, add 3.75mL of octadecene, and take 0.2g of octadecylamine and tri-n-octyl phosphorus oxide in the flask; ℃, after keeping for 9min, continue to heat up to 210℃; calculate the Cd needed to prepare each layer of quantum dots 2+ , Zn 2+ , S 2- The amount, dropwise added the special Cd, Zn, S shell precursor solution; prepared CdSe / CdS / Cd 0.4 Zn 0.6 S / ZnS quantum dots were centrifuged and purified twice with acetone, and then stored in a sealed, dark place at low temperature.

[0034] (2) Polyethylacrylic acid, heptylamine and coupling agent EDC.HCl are mixed and dissolved in dimethylformamide, wherein the molar ratio of polyethylacrylic acid to heptylamine is 1:30, and the molar ratio of coupling agent to heptylamine 1.25:1, and reacted for 10 hours to obtain polyethylacrylic acid-heptylamine whose long chain is polyacrylic acid homopolymer A.

[0035] (3) CdSe / CdS / Cd 0.4 Zn 0.6 S / ZnS core / shell quantu...

Embodiment 3

[0039] (1) Take 2.25mL of CdSe nuclear quantum dot chloroform solution, add 4mL of octadecene, and take 0.25g of octadecylamine and tri-n-octylphosphorus oxide in the flask; after argon gas for 35min, heat to 100°C , after keeping for 9min, continue to heat up to 220°C; calculate the Cd needed to prepare each layer of quantum dots 2+ , Zn 2+ , S 2- The amount, dropwise added the special Cd, Zn, S shell precursor solution; prepared CdSe / CdS / Cd 0.4 Zn 0.6 S / ZnS quantum dots were centrifuged and purified twice with acetone, and then stored in a sealed, dark place at low temperature.

[0040] (2) Polymethacrylic acid, octylamine and coupling agent EDC.HCl are mixed and dissolved in dimethylformamide, wherein the molar ratio of polymethacrylic acid to octylamine is 1:50, and the molar ratio of coupling agent to octylamine 1.75:1, and reacted for 10 hours to obtain polymethacrylic acid-octylamine whose long chain is polyacrylic acid homopolymer A.

[0041] (3) CdSe / CdS / Cd 0.4 ...

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Abstract

The invention relates to amphiphilic macromolecular modified oil-soluble nuclear / shell quantum dots and a preparation method. A nuclear layer is of CdSe quantum dots; and a shell layer comprises CdS, an alloy layer, ZnS, an amphiphilic polymer layer from the inside to the outside in turn. The structure of the alloy layer is: Cd0.4Zn0.6S, Cd0.45Zn0.55S or Cd0.6Zn0.4S; the structure of the amphiphilic polymer layer is that: an inner layer is an alkyl chain hydrophobic layer; a connecting layer is aliphatic long carbon chains; and an outer layer is a carboxyl hydrophilic layer; and the particle size range of the quantum dots is between 200 and 1,000 nm. By covering different shell layers with appropriate thickness on the surface of the CdSe nuclear quantum dots, the nuclear / shell quantum dots with high fluorescence efficiency and stable fluorescent properties are synthesized; by performing self-assembly water-solubility modification on self-made amphiphilic polymer and amphiphilic polymer, a formed amphiphilic polymer layer protects the surface structure and fluorescence properties of the nuclear quantum dots, can restrain cadmium ions and selenium ions from diffusing outwards and reduces the toxicity of the quantum dots to organisms; and the modified quantum dots cannot generate fluorescence resonance energy transfer in multi-flux detection.

Description

technical field [0001] The invention relates to the field of nanomaterial preparation and biochemical multi-flux detection, in particular to an amphiphilic polymer modified oil-soluble core / shell quantum dot and a preparation method thereof. Background technique [0002] Quantum dots (Quantum Dots, QDs), due to their unique optical and electrical properties, have attracted widespread attention from scientists and have become a bright spot in nanotechnology. With the continuous improvement of preparation technology, quantum dots have shown more and more broad application prospects in the biological field, especially as fluorescent probes for biomarkers, biodetection, and bioimaging. Compared with organic fluorescent molecules, quantum dots have many unique optical properties: their emission peak wavelength can be adjusted by the composition material and particle size, their excitation light wavelength range is very wide, they have a large Stokes shift and narrow symmetry. Fl...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C09K11/88C09K11/02
Inventor 常津朱盛疆张琦李新佳宫晓群宋涛张兵波成靖杨秋花崔叶郭伟圣
Owner 南通药享科技有限公司
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