Dual-stage stimulation-response type porphyrin MOF-aluminum oxide nano-composite fluorescent probe for phosphate radical detection
An alumina nanometer and fluorescent probe technology is applied in the field of chemical analysis and detection, which can solve the problems of alkalization and desertification, death of animals and plants, and inability to absorb calcium, and achieves the effects of rapid response, simple and rapid operation, and universality.
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[0039] A dual-stage stimulus-responsive porphyrin MOF@alumina nanocomposite fluorescent probe PMOF@Al 2 O 3 preparation methods, including:
[0040] A layer of aluminum oxide film is attached on the surface of PMOF by in-situ growth method, that is, it is obtained.
[0041] In some embodiments, the specific steps of the in-situ growth method are:
[0042] Mix PMOF, aluminum salt, organic solvent and water evenly to obtain a mixed solvent;
[0043] The benzoic acid is dissolved in the organic solvent, then added to the mixed solvent, mixed evenly, hydrothermally reacted, collected and precipitated, and dried.
[0044] In some embodiments, the mass ratio of the PMOF and the aluminum salt is: 1.6-2: 3.75-4.
[0045] In some embodiments, the condition of the hydrothermal reaction is to react at 90°C to 95°C for 4 to 6 hours.
Embodiment 1
[0048] like figure 1 , the schematic diagram of the synthesis principle of the fluorescent probe of the present invention: firstly, the 2D nanosheet Zr-BTB is synthesized, then the 2D nanosheet Zr-BTB binds TCPP molecules through coordination, and finally a dense layer of oxide is attached to its surface by the in situ growth method. Al thin films, resulting in a water-stable MOFs nanocomposite, namely PMOF@Al 2 O 3 . The method comprises the following steps: the synthesis method of the 2DZr-BTB nanosheet is: in a 50mL polytetrafluoroethylene lined reaction kettle, add ZrCl 4 (50mg), H 3 BTB (50mg), Benzoic acid (3g), H 2 A mixture of O (2.5 mL) and DMF (15 mL). The reaction kettle was sealed and placed in an oven at 120 °C for 48 h. The reaction kettle was taken out and slowly cooled to room temperature in the air. The product was collected by centrifugation. Finally, the 2D Zr-BTB was placed in a constant temperature drying oven for drying. Synthesis of PMOF: 2D Zr-BTB...
Embodiment 2
[0050] The probes prepared above were detected, and scanning electron microscopy ( figure 2 ) and transmission electron microscopy ( image 3 ) indicates that the probe has a good morphology.
[0051] Phosphate detection was performed on the fluorescent probe prepared above:
[0052] (1) Weigh 1mg PMOF@Al 2 O 3 Add to 1mL of water, the concentration is 1mg / mL, take 25μL PMOF@Al with a concentration of 1mg / mL 2 O 3 Add 2 mL of water and shake well.
[0053] (2) Add 20 μL of different interfering substances (K + , Na + , Mg 2+ , Ca 2+ , Cl - , CO 3 2- , SO 4 2- , HS - , NO 2 - , NO 3 - , Ac - , H 2 O 2 , GSH), incubate for 15min, centrifuge, take the supernatant to fix the excitation wavelength at 420nm, and test the supernatant fluorescence. from Figure 4 It can be seen that the fluorescent nanoprobe has good selectivity for phosphate.
[0054] Determination of the relationship curve between fluorescence intensity and phosphate concentration ( Figur...
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