Rhodamine fluorescent probe capable of detecting and separating heavy metal ions, and preparation method of rhodamine fluorescent probe
A technology of heavy metal ions and fluorescent probes, used in fluorescence/phosphorescence, alkali metal compounds, chemical instruments and methods, etc.
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Embodiment 1
[0023] Embodiment 1, the synthesis of rhodamine lactam (SRhB)
[0024] RhB (10.46mmol) was dissolved in 180ml absolute ethanol, N 2 Quickly add 40.23mL of ethylenediamine under the atmosphere, slowly add the temperature to 85°C, react for 24h, and distill under reduced pressure, the obtained powder is distilled with CH 2 Cl 2 (100mL) was dissolved, extracted with water (200mL), the organic layer was separated, washed with water 5 times, and distilled under reduced pressure to obtain an orange powder. Chromatography on silica gel (CH 2 Cl 2 / EtOH / Et 3 N=5:1:0.1) purification, yield 90%.
Embodiment 2
[0025] Embodiment 2, the preparation of azobenzene-rhodamine (SRhB-Azo)
[0026]Add 100mg maleic anhydride (MAH), 516mg SRhB, 20mg DMAP, 5mL DMSO to a 50mL one-necked flask, react at room temperature for 12 hours, add 191mg EDC, 137mg HOBt, activate for 1 hour, add 197.24mg azobenzene (Azo) and react at room temperature for 12 hours . The resulting powder was washed with CH 2 Cl 2 (100mL) was dissolved, extracted with water (200mL), separated the organic layer, and distilled under reduced pressure to obtain a pink powder, which was purified by silica gel chromatography (CH 2 Cl 2 ).
Embodiment 3
[0027] Embodiment 3, detect mercury ion
[0028] Configure 2.5×10 in a 100mL volumetric flask -3 M's SRhB-MAH-A 2 O ethanol standard solution, 1×10 -4 M mercury ion standard solution. Take 1mL of SRhB-Azo standard solution and 0.1mL, 0.2mL, 0.4mL, 0.6mL, 0.8mL, 1.0mL of mercury ion standard solution in a centrifuge tube, dilute to 5mL with ethanol, measure the fluorescence intensity at 492nm, and carry out at 563nm Photometry.
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