A kind of acylhydrazone zinc complex fluorescent probe and its preparation method and application
A technology of fluorescent probes and complexes, applied in the field of chemical analysis, can solve the problems of cumbersome and complicated operation, long time-consuming, high detection cost, etc., and achieve the effects of cheap reaction, simple operation and shortened detection period.
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Embodiment 1
[0035] This embodiment provides a fluorescent probe for the zinc acylhydrazone complex, the molecular formula of the zinc acylhydrazone complex is [Zn(C 13 h 9 N 3 o 3 )(H 2 O)·2C 3 h 7 NO] n ; where C 13 h 9 N 3 o 3 2,4-dihydroxybenzaldehyde isonicotinoyl hydrazone, C 3 h 7 NO is N,N-dimethylformamide. Wherein, n is an integer greater than or equal to 1.
[0036] The asymmetric unit of the acylhydrazone zinc complex contains one zinc ion, one molecule of 2,4-dihydroxybenzaldehyde isonicotinoyl hydrazone, one molecule of coordination water and two free molecules of DMF.
[0037] Such asfigure 1 As shown, the zinc ions respectively react with O3, N1, O2 in one molecule of 2,4-dihydroxybenzaldehyde isonicotinoyl hydrazone, one molecule of O1W in coordination water, and the other two molecules of 2,4-dihydroxybenzaldehyde N3A and O2B in isonicotinoyl hydrazone form a coordination bond, and zinc ions form an octahedral configuration.
[0038] Such as figure 2 As s...
Embodiment 2
[0041] This embodiment provides a method for preparing a fluorescent probe of an acylhydrazone zinc complex, which includes the following steps:
[0042] A. Dissolve isoniazid in ethanol, and add the ethanol solution of 2,4-dihydroxybenzaldehyde dropwise into the ethanol solution of isoniazid after heating to reflux; ℃, stirring and reacting for 10-12 hours to obtain the reaction solution;
[0043] B. Take the reaction solution in step A, and after vacuum filtration, recrystallize the solid obtained by vacuum filtration with anhydrous methanol to obtain 2,4-dihydroxybenzaldehyde isonicotinoyl hydrazone;
[0044] C. Dissolve the 2,4-dihydroxybenzaldehyde isonicotinoyl hydrazone in step B in 10~15mL N,N-dimethylformamide, and add it to a 25ml colorimetric tube; then, add 5mL in turn Buffer layer solution and 10-15mL of Zn(NO 3 ) 2 ·6H 2 O methanol solution; wherein, 2,4-dihydroxybenzaldehyde isonicotinoyl hydrazone DMF solution and Zn(NO 3 ) 2 ·6H 2 [Zn(C 13 h 9 N 3 o ...
Embodiment 3
[0054] [Zn(C 13 h 9 N 3 o 3 )(H 2 O)·2C 3 h 7 NO] n The structure was characterized, proving that the target compound was synthesized.
[0055] Infrared characterization as image 3 Shown, [Zn(C 13 h 9 N 3 o 3 )(H 2 O)·2C 3 h 7 NO] n at 3328cm -1 A broad peak appears nearby, which can be identified as the characteristic peak of ν(O-H), which is consistent with the experimental fact that a phenolic hydroxyl group in the complex has not been deprotonated. Complex at 1600.5cm -1 The characteristic peak of ν(C=N) appears, and the ν(C=N) of the ligand appears at 1609cm -1 , the two have a more obvious red shift after coordination; the ligand is at 1647cm -1 The characteristic peak of ν(C=O) disappears after forming the complex, and at 1361cm -1 A characteristic peak of the enol formula ν(C–O) appears.
[0056] The X-ray powder diffraction characterization results are as follows: Figure 4 As shown, by [Zn(C) prepared in Example 2 13 h 9 N 3 o 3 )(H 2 O)·2...
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