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Fluorescence-enhanced probe compound preparation method and trivalent chromium ion detection method

A technology of fluorescent probes and compounds, applied in the field of fluorescent probes, can solve the problems of complex design and synthesis of fluorescent probes, low fluorescence quantum yield, low detection limit, etc., and achieve high stability and selectivity of probe products. and high sensitivity, simple pre-processing effect

Inactive Publication Date: 2015-08-12
UNIV OF JINAN
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] Prior art CN103387830A provides a chromium ion fluorescent probe compound and its preparation method, but the design and synthesis of the fluorescent probe is complicated, the fluorescence quantum yield is not high, and the detection limit is not low enough, so it is difficult to achieve current scientific research and practical application requirements

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  • Fluorescence-enhanced probe compound preparation method and trivalent chromium ion detection method
  • Fluorescence-enhanced probe compound preparation method and trivalent chromium ion detection method
  • Fluorescence-enhanced probe compound preparation method and trivalent chromium ion detection method

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Embodiment 1

[0033] Embodiment 1, Synthetic experiment of intermediate product II

[0034] Take 0.31 g of cyanobiphenol and 0.22 g of anhydrous magnesium chloride and put them in a flask under nitrogen protection, add 0.61 g of anhydrous triethylamine and 20 ml of acetonitrile, stir to make them evenly mixed, add 0.66 g of paraformaldehyde, and heat to reflux 6 hours. After the reaction was stopped, a small amount of water was added to quench it, acidified with excess dilute hydrochloric acid, the mixture was extracted 3 times with ethyl acetate, dried, and purified by silica gel column to obtain product II. H NMR spectrum: 1 H NMR (400 MHz, CDCl 3 ) δ ppm : 11.11 (s, 1H), 9.99 (s, 1H), 7.78 (m, 4H), 7.66 (dt, 2H, J=8.55, 1.99), 7.12 (d, 1H, J=8.46).

Embodiment 2

[0035] Embodiment 2, Synthesis experiment of intermediate product Ⅲ

[0036] Take 1.1 grams of sample II, 0.82 grams of 2-chloromethylpyridine hydrochloride, 2.5 grams of anhydrous potassium carbonate, and 0.36 grams of potassium iodide, put them together in a flask, and add 35 milliliters of acetonitrile to dissolve them. After heating to reflux for 6 hours, the reaction was stopped, and the inorganic salt was removed by filtration. The obtained crude product was concentrated and purified on a silica gel column to obtain product III. H NMR spectrum: 1 H NMR (400 MHz, CDCl 3 ) δ ppm : 10.65 (s, 1H), 8.64 (d, 1H, J=4.42), 8.12 (d, 1H, J=2.53), 7.78 (m, 2H), 7.73 (d, 2H, J=8.58) , 7.67 (dd, 2H, J=8.66, 2.25), 7.55 (d, 1H, J=8.06), 7.29 (dd, 1H, J=7.62, 5.28), 7.18 (d,1H, J=8.74), 5.39 (s, 2H).

Embodiment 3

[0037] Embodiment 3, Synthesis experiment of fluorescent probe I of the present invention

[0038] Take 0.04 g of phenanthrenequinone and 0.16 g of ammonium acetate in 15 ml of ethanol, and then add 1.5 ml of dichloromethane. After complete dissolution, cool slightly, add sample III and a drop of acetic acid. After reacting for 2 hours, filter with suction and wash with ethanol to obtain the product probe Ⅰ. H NMR spectrum: 1 H NMR (400 MHz, CDCl 3) δ ppm : 12.97 (s, 1H), 9.00 (t, 2H, J=2.49), 8.34 (d, 1H, J=7.65), 8.79 (d, 1H, J=7.97), 8.74 (d, 1H, J=8.18), 8.39 (d, 1H, J=7.65), 7.55-7.90 (m, 10H), 7.42-7.48 (m, 2H), 7.24 (d, 1H, J=8.64), 5.53 (s, 2H ).

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Abstract

The invention relates to a novel fluorescence-enhanced probe compound preparation method and a trivalent chromium ion detection method. The chromium ion fluorescence-enhanced probe compound has a structure shown in the formula I. The preparation method comprises mixing 4'-Hydroxy-4-biphenylcarbonitrile, anhydrous magnesium chloride and anhydrous triethylamine in an acetonitrile solvent in a nitrogen protective atmosphere, adding paraformaldehyde into the mixture, carrying out reflux to obtain an intermediate product, carrying out reflux on the intermediate product, 2-chloropyridine hydrochloride, anhydrous potassium carbonate and potassium iodide in an acetonitrile solvent to obtain a second intermediate product, mixing the second intermediate product, phenanthraquinone and ammonium acetate in an ethanol solvent, and carrying out a reaction process in the presence of acetic acid as a catalyst to obtain a desired product probe. The fluorescence-enhanced probe compound has good selectivity and sensitivity to trivalent chromium ions and has a fast response speed. The trivalent chromium ion detection method has a simple sample pretreatment process and is suitable for detection of a trace amount of trivalent chromic ions in water and in the environment.

Description

technical field [0001] The invention relates to the preparation of a novel fluorescent probe compound and the detection of trivalent chromium ions, belonging to the technical field of fluorescent probes. technical background [0002] Heavy metals and transition metals widely exist in nature, but a large amount of enrichment often causes serious heavy metal pollution to the environment and organisms. Chromium ions, as one of the essential trace elements for the human body, play an important role in the normal metabolism of the human body. For example, chromium ions can also prevent genetic mutations in intracellular genetic material, regulate carbohydrate and lipid metabolism, and reduce blood cholesterol and triglyceride levels. Chromium deficiency can easily lead to serious diseases such as arteriosclerosis and diabetes. On the contrary, excessive intake of chromium can cause poisoning, causing kidney, liver, nervous system and other lesions. In industry, chromium and i...

Claims

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Application Information

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IPC IPC(8): C09K11/06C07D401/12G01N21/64
Inventor 范春华黄曦明齐俊杰吕正亮张瑞雪杨荣张新明
Owner UNIV OF JINAN
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