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Gold ion probe and its preparation method and application

A technology of gold ions and probes, which is applied in the field of gold ion probes and its preparation and application, can solve the problems of difficult operation, long analysis time, expensive instruments, etc., and achieve good selectivity and specificity, and large pH changes The scope and the effect of simple and easy preparation process

Active Publication Date: 2016-06-15
NANJING TECH UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, most of these methods take a long time to analyze, and the required instruments are expensive and not easy to operate

Method used

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  • Gold ion probe and its preparation method and application
  • Gold ion probe and its preparation method and application
  • Gold ion probe and its preparation method and application

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Embodiment 1 prepares gold ion fluorescent probe

[0025] Dissolve 200mg of 4,5-fluorescein bisaldehyde in 40ml of ethanol solution, and slowly add 5ml of methanol solution containing 112mg of hydrazinopyridine dropwise within 30min; under the protection of nitrogen, react at room temperature for 12 hours; after the reaction, The reaction product was precipitated out, filtered, and the obtained solid was dried in a vacuum oven to obtain a crude product; washed with n-pentane to obtain 170 mg of a light pink solid, which was the pure gold ion fluorescent probe ( 1 H-NMR chart and high-resolution mass spectrogram see Image 6 , Figure 7 ). The measured molecular weight of the obtained pure fluorescent probe is 570.

[0026] Present embodiment process route:

[0027]

Embodiment 2

[0028] Embodiment 2 makes the spectral properties of gold ion fluorescent probe reacting with various ions

[0029] Weigh 5.7 mg of the gold ion fluorescent probe prepared in Example 1, and prepare 10 mL of DMSO solution with a concentration of 1 mM as the mother solution.

[0030] Fluorescence spectrum test: Add 30μL of the above mother solution into a certain amount of 10mM HEPES buffer solution (pH7.4), and then add various ions: Zn 2+ , Li 2+ ,Cs 2+ , Fe 2+ ,Co 2+ , Ag + ,Cd 2+ , Ni 2+ , Fe 3+ , K + ,Pb 2+ ,Au + ,Cu 2+ , Na + ,Mg 2+ , Ca 2+ ,Cr 3+ ,Hg 2+ ,Al 3+ ,Zr 4+ ,Mn 2+ ,NH 4 + The final concentration of ions was 100 μM, and the final concentration of fluorescent probe was 10 μM. The fluorescence emission spectrum was tested immediately under the excitation light wavelength of 493nm. The slit width for excitation and emission is 1.5 / 3.0nm. The result is as figure 1 shown. The solution prepared above was irradiated with a 365nm ultraviolet lam...

Embodiment 3

[0034] Embodiment 3 makes the spectroscopic property of gold ion fluorescent probe and gold ion reaction product

[0035] Add 30 μL of the mother liquor in Example 2 to a certain amount of 10 mM HEPES buffer solution (pH 7.4), and then add different equivalents of gold ions so that the final concentration of the fluorescent probe is 10 μM, and the final concentrations of gold ions are 0 μM and 10 μM respectively , 20 μM, 30 μM, 40 μM, 50 μM, 60 μM, 70 μM, 80 μM, 90 μM, 100 μM, 110 μM, 120 μM, 130 μM, 140 μM, 150 μM, 160 μM, 170 μM, 180 μM, 190 μM, 200 μM, 250 μM, 300 μM. Immediately after the addition of ions, their fluorescence emission spectra were measured. The fluorescence emission spectrum is excited at 493nm; the slit width of excitation and emission is 1.5 / 1.5nm. The resulting fluorescence increment graph is shown in image 3; Make a working curve with the fluorescence intensity data at 523nm, the results are shown in Figure 4 .

[0036] The experimental results sh...

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Abstract

The invention discloses a gold ion fluorescence probe, a preparation method and an application thereof. The fluorescence probe has high selectivity and high sensitivity, can be used for detecting gold ions. The gold ion fluorescence probe is a 4,5-dihydrazine pyridyl fluorescein derivative shown in a formula I, the preparation method comprises the following steps of reacting 4,5-fluorescein bi-aldehydes and hydrazinopyridines in an ethanol solution to generate the dihydrazine pyridyl fluorescein derivative which can be taken as the gold ion fluorescence probe.

Description

technical field [0001] The invention relates to a gold ion fluorescent probe and its preparation method and application. Background technique [0002] Gold, a precious metal, has played an important role in human life since before recorded history. Due to its unique physical and chemical properties, it has been widely used in various fields such as electronic materials, catalysts, medicine, and sensors. For example, gold ions have been successfully used as catalysts in the activation of carbon-carbon triple bonds, and gold complex drugs are commonly used in the treatment of rheumatoid arthritis, tuberculosis, tumors and other diseases. Colorimetric and fluorescent sensors based on gold nanoparticles have also been extensively reported in recent years. Although widely used, the toxicity of gold ion itself cannot be ignored. Studies have shown that gold ions can combine with DNA and cause DNA strand breaks, and enrichment in organisms will cause damage to the liver, kidneys...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D493/10G01N21/64C09K11/06
Inventor 陈小强王碧慧王苏鲁
Owner NANJING TECH UNIV
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