A fluorescent molecular probe for detecting mercury ions and its preparation method and application
A technology of fluorescent molecular probes and mercury ions, which is applied in the field of fluorescent probes to achieve short response time, good selectivity, and good recognition effects
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[0050] A preferred embodiment of the present invention provides a method for preparing a fluorescent molecular probe for detecting mercury ions, the specific steps are as follows:
[0051] (1) Weigh 4.00g of 4-bromo-1,8-naphthalene dicarboxylic anhydride into a 250mL three-necked flask, add 120mL of absolute ethanol, then add 8mL of aniline, slowly inject nitrogen gas for 10 minutes, and place in an oil bath Stir and heat to reflux for 7 hours. Thin-layer chromatography (TLC) was used to confirm that the reactants were completely reacted and the reaction was stopped. Take it off and let it stand overnight, and filter to obtain the light yellow product N-phenyl-4-bromo-1,8-naphthalimide (PBN). The filtrate was concentrated to obtain the light yellow product N-phenyl-4-bromo-1,8-naphthoimide (PBN).
[0052] The product N-phenyl-4-bromo-1,8-naphthalimide (PBN) was 3.33g, the yield was 83.3%, and the melting range was 188°C-190°C. IR(KBr)550cm -1 、700cm -1 、770cm -1 、885cm ...
experiment example 1
[0058] The N-phenyl-4-bromo-1,8-naphthalimide (PBN) prepared in the example was characterized by infrared spectroscopy. like figure 1 Shown, the main characteristic peak of infrared spectrogram is IR (KBr): V=550cm -1 It is C-C=O peak, 700cm -1 、770cm -1 It is the C-H peak of naphthalene ring, 885cm -1 Br peak on naphthalene ring, 1070cm -1 It is C=O peak, 1193cm -1 、1379cm -1 、1430cm -1 It is the characteristic peak of benzene ring skeleton, 1530cm -1 It is N-H peak, 1656cm -1 It is amide N-C=O peak, 3078cm -1 It is a benzene ring peak, which is consistent with the literature value and thus confirms that the functional group of the product is correct.
[0059] The structure of p-N-phenyl-4-(N,N-dihydroxyethyl)amino-1,8-naphthalimide (PDAN) was characterized by infrared spectroscopy. like figure 2 Shown, the main characteristic peak of infrared spectrogram is IR (KBr): v=3182cm -1 For -CH2 peak, 1678cm -1 It is N-C=O peak in amide, 2930cm -1 It is C-H peak, 159...
experiment example 2
[0065] N-phenyl-4-(bis(ethylthioethyl)amino)-1,8-naphthalimide is formulated with anhydrous ethanol: deionized water = 2:1 to a concentration of 1.0x10 -5 mol / L solution. Hg 2+ 、Cu 2+ 、Cr 3+ 、Co 2+ , Ca 2+ 、K + 、Na + 、Ba 2+ The salt of other metal ions is made into 1.0x10 with deionized water -1 mol / L solution.
[0066] Determination of ultraviolet-visible absorption spectrum and fluorescence spectrum: Pour the prepared solution into a cuvette, absolute ethanol: deionized water = 2:1 solvent as a reference solution, on the TU-1810PC ultraviolet-visible spectrophotometer Test the ultraviolet-visible absorption spectrum, test the fluorescence spectrum on a fluorescence spectrophotometer, and the temperature is room temperature.
[0067] In the UV spectrum of N-phenyl-4-(bis(ethylthioethyl)amino)-1,8-naphthalimide as Figure 7 As shown, the fluorescence spectrum as Figure 8 As shown, it can be observed that Ca 2+ 、Ba 2+ 、Co 2+ 、Cu 2+ 、K + , Mg 2+ 、Na + 、Ni 2+...
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