Fluorescent probe for divalent mercury ion and temperature detection, preparation method and application thereof
A fluorescent probe, divalent mercury technology, used in chemical instruments and methods, thermometers, fluorescence/phosphorescence, etc., can solve the problems of insufficient sensitivity, high cost, and insufficient probe selectivity, and achieve high sensitivity, overcome The effect of error and signal stability
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[0034] The preparation method of the fluorescent probe for divalent mercury ion and temperature detection comprises the following steps:
[0035] Step 01. Synthesis of 3-(piperazine)-rhodamine B hydrazide (1), including the following steps:
[0036] (1) Take a dry 100 ml two-neck bottle, replace the inside of the bottle with nitrogen, add m-hydroxyphenylpiperazine (1.78g, 10.0 mmol), 2-(4-diethylamino)-2-hydroxy)- Benzoic acid (3.13 g, 10.0 mmol) and trifluoroacetic acid (20 mL) were heated to reflux and stirred for 24 h, and then the organic solvent was distilled off under reduced pressure to obtain a red residue;
[0037] (2) Add ethanol (30 mL) and ethylenediamine (15 mL), heat and reflux and stir for 6 h. After the reaction is complete, remove ethanol and unreacted ethylenediamine by vacuum distillation, add the water phase, and Chloromethane extraction, combined organic phases (extracted three times, total about 250 mL), anhydrous MgSO 4 dried, filtered, concentrated; ...
Embodiment 2
[0042] Example 2, Research on the Recognition Performance of BR Fluorescent Probes to Mercury Ions
[0043] 1. Study on the selectivity of BR fluorescent probes to mercury ions
[0044] Prepare BR with anhydrous methanol (10 -3 mol L -1 ) stock solution, and ultrapure water to prepare Ag + 、Ba 2+ , Ca 2+ 、Cd 2+ 、Co 2+ 、Cu 2+ , Fe 2+ 、K + , Hg 2+ , Mg 2+ , Mn 2+ 、Na + 、Ni + , Zn 2+ stock solution (10 -2 mol L -1 ), prepare 0.02 mol L -1 HEPES buffer (pH=7.2). First add a mixed solvent (V / V = 1:9) of HEPES buffer (250 μL) and anhydrous methanol (2230 μL) to the cuvette, and then add BR stock solution (20 μL) to detect the ultraviolet absorption spectrum of the BR solution and fluorescence emission spectrum, add ion stock solution (20 μL) respectively, detect its ultraviolet absorption spectrum and fluorescence emission spectrum (λex=520nm), and observe the corresponding situation of fluorescent probe BR to various cations.
[0045] figure 2 For BR (HEPES ...
Embodiment 3
[0064] Embodiment three, the detection of temperature by BR fluorescent probe
[0065] Prepare BR stock solution with anhydrous methanol (10 -3 mol L -1 ), deionized water to prepare Hg 2+ stock solution (10 -2 mol L -1 ). A mixed solvent (V / V = 1:9) of HEPES buffer (250 μL) and anhydrous methanol (2230 μL) was added to the cuvette, and then BR stock solution (20 μL) and Hg 2+ The stock solution (20 μL) was shaken evenly, and its fluorescence emission spectrum was detected at different temperatures (temperature range 10-45°C).
[0066] Such as Figure 13 As shown, with the increase of temperature, BR+Hg 2+ The fluorescence intensity of the system gradually weakened and showed a good linear relationship (R 2 = 0.99075), indicating that BR+Hg 2+ The system can be used for temperature detection.
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