Double-excitation fluorescence probe preparation and application in detection of hydrazine in water
A fluorescent probe, fluorescein technology, applied in the field of analytical chemistry, can solve problems such as liver central nervous system damage, and achieve the effect of low cost
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Embodiment 1
[0034] Embodiment 1 Novel dual excitation fluorescent probe Tb III -dtpa-bis(fluorescein)
[0035] (1) Preparation method
[0036] 1, the preparation of diethylenetriaminepentaacetic dianhydride (dtpaa)
[0037] Weigh 7.8100g (0.02mmol) of dtpa, 16.0mL (0.08mmol) of acetic anhydride, and 10.0mL (0.12mmol) of pyridine into a three-necked round bottom flask, mix well, and heat with stirring at 65°C for 24h. Cool to room temperature, filter the reaction mixture, wash twice with a small amount of acetic anhydride and anhydrous ether, filter with a vacuum pump, and dry the resultant in a vacuum oven at 80°C to obtain dtpaa.
[0038] 2. Preparation of diethylenetriaminepentaacetic acid difluorescein (dtpa-bis (fluorescein))
[0039]Take 1.9610g of dtpaa (5.5mmol), 8.0mL (16.5mmol) of triethylamine, anhydrous DMF (50mL), and 1.6515g (11mmol) of fluorescein in a three-neck round bottom flask, and mix well. Heating at a constant temperature of 100°C and stirring rapidly for 24 hour...
Embodiment 2
[0047] Embodiment 2 Double excitation fluorescent probe Tb 3+ -Application of dtpa-bis(fluorescein) in detection of hydrazine
[0048] 1. Fluorescence spectra of dual-excitation fluorescent probe hydrazine detection
[0049] Experimental conditions: Take a certain amount of hydrazine (N 2 h 4 ) was prepared with distilled water to a concentration of 1.0×10 -3 mol / L solution as a hydrazine stock solution.
[0050] Take 5.0 mL of the hydrazine stock solution in a 50 mL volumetric flask, and then add 5.0 mL of the dual-excitation fluorescent probe stock solution prepared in Example 1, and use buffer to make up the volume. At this time, the probe concentration was 5.0×10 -5 mol / L, the concentration of each detected substance is 1.0×10 -4 mol / L. Changes in fluorescence spectra were observed at excitation wavelengths of 247 nm and 500 nm.
[0051] The result is as Figure 5a , Figure 5b shown. Such as Figure 5a As shown, under the excitation of 247nm, the fluorescent p...
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