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Preparation method of functionalized graphene quantum dots producing ultrasensitive fluorescence response to Fe<3+>

A graphene quantum dot and fluorescence response technology, which is applied in the chemical industry to achieve the effects of good selectivity, high stability and enhanced fluorescence intensity

Inactive Publication Date: 2017-05-10
JIANGNAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, iron supplement health care products may be in contact with air during production and transportation, resulting in Fe 2+ is oxidized to form Fe 3+

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Weigh 2g of citric acid and 1.4g of D-penicillamine in a beaker, add 30mL of twice distilled water and stir until dissolved, transfer the mixed solution in the beaker to a 50mL autoclave, and react at a temperature of 200°C for 2.5 h. The obtained graphene quantum dot solution was freeze-dried, and the graphene quantum dot solution obtained by freeze-drying was prepared with double distilled water with a mass concentration of 0.2 mg / mL. Take 200 μL graphene quantum dot solution, 200 μL Fe 3+ Shake the sample solution and 0.6 mL of BR buffer solution with pH=2, react at room temperature for 10 min, and measure the fluorescence intensity at the emission wavelength when the excitation wavelength is 356 nm on a fluorescence spectrophotometer. Method for Fe 3+ The detection limit is 1.3×10 -7 M.

Embodiment 2

[0026] Weigh 2g of citric acid and 0.02g of D-penicillamine in a beaker, add 30mL of twice distilled water and stir until dissolved, transfer the mixed solution in the beaker to a 50mL autoclave, and react at a temperature of 180°C for 2h . The obtained graphene quantum dot solution was freeze-dried, and the graphene quantum dot solution obtained by freeze-drying was prepared with double distilled water with a mass concentration of 0.1 mg / mL. Take 200 μL of graphene quantum dots, 200 μL of Fe 3+ Shake the sample solution and 0.6 mL of BR buffer solution with pH=5, react at room temperature for 5 min, and measure the fluorescence intensity at the emission wavelength when the excitation wavelength is 356 nm on a fluorescence spectrophotometer. Method for Fe 3+ The limit of detection is 2×10 -6 M.

Embodiment 3

[0028] Weigh 2 g of citric acid and 3.2 D-penicillamine in a beaker, add 30 mL of double distilled water and stir until dissolved, transfer the mixed solution in the beaker to a 50 mL autoclave, and react at 250°C for 5 hours. The obtained graphene quantum dot solution was freeze-dried, and the graphene quantum dot solution obtained by freeze-drying was prepared with double distilled water with a mass concentration of 0.5 mg / mL. Take 200 μL of graphene quantum dots, 200 μL of Fe 3+Shake the sample solution and 0.6 mL of BR buffer solution with pH=1.81, react at room temperature for 3 min, and measure the fluorescence intensity at the emission wavelength when the excitation wavelength is 356 nm on a fluorescence spectrophotometer. Method for Fe 3+ The detection limit is 3×10 -6 M.

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Abstract

The invention belongs to the field of chemical industry and relates to a preparation method of functionalized graphene quantum dots producing ultrasensitive fluorescence response to Fe<3+>. Citric acid and a certain mole ratio of penicillamine are put in a beaker and are dissolved in water to form a mixed acid solution; the obtained mixed acid solution is transferred to a high-pressure reaction kettle, heating reaction and freeze drying are performed to obtain the functionalized graphene quantum dots; the functionalized graphene quantum dots are dissolved in water to obtain a graphene water solution; a buffer solution is mixed with a Fe<3+>-containing solution and reacts with the prepared functionalized graphene quantum dot water solution for a certain time, then the fluorescence intensity is determined on a fluorescence spectrophotometer, and the Fe<3+> content in a sample is calculated on the basis. The citric acid and the penicillamine are used as a mixed carbon source to prepare the functionalized graphene quantum dots through one-step hydrothermal reaction, remarkable fluorescence quenching is produced by utilizing specific combination between the Fe<3+> and the quantum dots, and high sensitivity and high-selectivity determination conducted on Fe<3+> in iron supplementing health care products is achieved.

Description

technical field [0001] The invention belongs to the field of chemical industry and relates to a 3+ Preparation method of functionalized graphene quantum dots with ultrasensitive fluorescence response. Background technique [0002] Graphene quantum dots have the characteristics of good chemical stability, excellent photoelectric properties, low toxicity and light resistance, and are widely used in many aspects such as sensors, nanomaterial preparation and biological imaging (F.X.Wang, Z.Y.Gu, W.Lei , W.J.Wang, X.F.Xia, Q.L.Hao, Graphene quantum dots as a fluorescent sensing platform for highly efficient detection of copper(II)ions, Sens. Actuators B190(2014) 516-522). At present, the preparation methods of graphene quantum dots mainly include top-down synthesis method and bottom-up synthesis method. The former is to cut micron-scale graphene oxide sheets into nano-scale graphene quantum dots by oxidation. This method is not only time-consuming and the yield is low, but als...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B32/184G01N21/64C09K11/65
CPCG01N21/6428C09K11/65G01N2021/6432
Inventor 李在均汪漩卿思荔
Owner JIANGNAN UNIV
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