Preparation and application of novel fluorescent probe and test paper for hydrazine hydrate detection
A fluorescent probe, hydrazine hydrate technology, applied in the field of analytical chemistry, can solve the problems of inability to adapt to the market demand for rapid detection, requiring tens of minutes or even hours, and low detection accuracy, achieving fast response, low cost, Sensitive effect
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Embodiment 1
[0042] Synthesis and structural characterization of compound 2 (ethyl 7-hydroxy-2-oxo-2H-chromene-3-carboxylate)
[0043] Dissolve 2,4-dihydroxybenzaldehyde (2.76 g, 20 mmol) in 10 mL of absolute ethanol at room temperature, add diethyl malonate (6.40 g, 40 mmol) and piperidine 20 mmol, heat up to 90 oC under reflux, TLC monitoring reaction until complete. After the reaction was taken down and allowed to cool, absolute ethanol was removed by rotary evaporation, and the remaining liquid was dropped into water drop by drop, and a large number of yellow solids were seen to precipitate. After suction filtration and washing of the filter cake, 3.76 g of a yellow solid product was obtained after drying, with a yield of 80.5%. 1 H NMR (400MHz, DMSO-d 6 ): δ (ppm) = 11.08 (s, 1H), 8.87 (s, 1H), 7.75 (d, J = 8.8 Hz, 1H),6.84 (dd, J 1 = 8.8 Hz, J 2 = 2.4 Hz, 1H), 6.72 (d, J = 2.4 Hz, 1H), 4.26 (q, J = 7.2 Hz, 2H), 1.30 (t, J = 7.2 Hz, 3H).
[0044] Synthesis and struct...
Embodiment 2
[0051] Preparation of fluorescent probe master solution
[0052] Accurately weigh 4.10 mg of the product obtained from the above separation with a purity of more than 99% and carefully transfer it to a 50 mL volumetric flask, add CH at room temperature 3 CN, shake well to dissolve it completely, and finally dilute to the mark to obtain 1 mM probe mother solution. During the test, 20 μL of the above solution was measured with a micro-injector each time, dissolved in the test system, and the total volume of each test was guaranteed to be 2 mL. At this time, the concentration of the fluorescent probe in the test system was 10 μL. μM.
Embodiment 3
[0054] Preparation of hydrazine hydrate mother liquor
[0055] Hydrazine hydrate was prepared into 5 mL stock solutions with different concentration gradients (0.1 mM, 0.2 mM, 0.4 mM, 0.7 mM, 1 mM, 1.5 mM, 2.0 mM, 2.5 mM, 3.0 mM, 3.5 mM, 4.0 mM) with PBS buffer solution. The small molecules and inorganic salts required for the remaining tests were respectively prepared into mother solutions with a concentration of 3 mM in PBS buffer solution.
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