An enhanced azo-salen Schiff base fluorescent probe, its synthesis and application
A fluorescent probe, enhanced technology, applied in the field of fluorescent probes, can solve the problems of large slope changes of curves, great influence on reagent purity, long reaction time, etc., achieve low detection limit, easy control of reaction conditions, and simple synthesis method Effect
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Embodiment 1
[0037] Example 1 Preparation and Characterization of Enhanced Azo-Salen Schiff Base Fluorescent Probe
[0038] Synthetic azo compounds:
[0039] Dissolve 1.5318g (10mmol) of 3,4-dimethoxyaniline and 2mL of concentrated hydrochloric acid in a 100mL round bottom flask with 15mL of distilled water, and then weigh sodium nitrite (NaNO 2 ) 2.4835g (12mmol), stir well and control the temperature at 0-5°C, and react for 30 minutes.
[0040] Add 1.7218 g (10 mmol) of 2-hydroxyl-1-naphthaldehyde in ethanol solution dropwise to the above solution, stir for 3 hours, add sodium carbonate (Na 2 CO 3 ) aqueous solution to adjust the pH to 7-8, let stand, filter with suction, and recrystallize from absolute ethanol to obtain 16 g of yellow solid powder, yield: 81.26%.
[0041] Synthetic fluorescent probes:
[0042] Dissolve 2.6989 g (8 mmol) of the yellow solid and 0.3606 g (4 mmol) of dihydrazide carbonate in absolute ethanol, add 2 to 3 drops of concentrated phosphoric acid, and stir a...
Embodiment 2
[0051] Embodiment 2 Enhanced azo-Salen Schiff base fluorescent probe detection method for metal ions
[0052] Mix various metal salts (aluminum nitrate, cobalt chloride, zinc acetate, lead nitrate, manganese acetate, ferric chloride, magnesium sulfate, cadmium sulfate, copper nitrate, chromium chloride, high mercury chloride, nickel nitrate) into 1×10 -4 mol / L aqueous solution. The enhanced azo-Salen Schiff base fluorescent probe was dissolved in acetonitrile to make 5×10 -4 mol / L standard solution. The method for measuring the fluorescence intensity of metal ions on the enhanced azo-Salen Schiff base fluorescent probe: add 0.1 mL of enhanced azo-Salen Schiff base standard solution and 5 mL of acetonitrile into the colorimetric tube, then add various metal ions respectively, and set Make up to 10mL, and measure the fluorescence intensity after 3 hours of reaction. The fluorescence excitation wavelength is 440nm, and the slit width is 10nm / 10nm.
Embodiment 3
[0053] Embodiment 3 Enhanced azo-Salen Schiff base fluorescent probe pair Al 3+ selective identification of
[0054] In order to investigate the effect of the enhanced azo-Salen Schiff base fluorescent probe on Al 3+ The selectivity of different metal ions (Al 3+ 、Co 2+ , Zn 2+ , Pb 2 , Mn 2+ , Fe 3+ , Mg 2+ 、Cd 2+ 、Cu 2+ 、Cr 3+ , Hg 2+ 、Ni 2+ ) in the presence of enhanced azo-Salen Schiff base fluorescence probe fluorescence emission spectrum (metal ion concentration is 1×10 -5 mol / L), see Figure 4 .
[0055] Depend on Figure 4 It can be seen that when Co 2+ , Zn 2+ , Pb 2 , Mn 2+ , Fe 3+ , Mg 2+ 、Cd 2+ 、Cu 2+ 、Cr 3+ , Hg 2+ 、Ni 2+ , the fluorescence intensity of the system has no obvious change, when adding Al 3+ After that, the fluorescence intensity of the system is greatly enhanced, which shows that the azo-Salen Schiff base has a strong effect on Al 3+ Produced a clear fluorescent response and good selective recognition, which can be used as...
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