Method for rapid and highly-selective detection of hypochlorous acid
A technology for qualitative detection of hypochlorous acid, applied in chemical instruments and methods, measuring devices, instruments, etc., can solve problems such as insufficient sensitivity, insufficient selectivity, complex synthesis, etc., and achieve simple synthesis, good stability, and reaction. responsive effect
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[0032] Example 1
[0033]
[0034] (Scheme 1) 290mg (1mmol) of azepine-4-chloro-1,8-naphthimide was dissolved in 15mL of acetonitrile, then 110mg (1mmol) of p-aminophenol was added, and then 326mg (1mmol) of cesium carbonate was added and refluxed for 2h , And then use high-pressure pump for suction filtration to obtain filtrate, which becomes our crude product. If a relatively pure product is to be obtained, the filtrate can be separated by a chromatographic column with a mixed system of dichloromethane and methanol (for example, v / v, 100:1) to obtain the pure product, 200 mg of the yellow pure product is obtained, and the yield is 50%.
[0035] (Scheme 2) Dissolve 290mg (1mmol) of azetyl-4-chloro-1,8-naphthimide in 15mL of acetonitrile, then add 220mg (2mmol) of p-aminophenol, and then add 652mg (2mmol) of cesium carbonate to reflux 4h, then use the high-pressure pump for suction filtration to obtain the filtrate, which becomes our crude product. If a relatively pure product is...
Example Embodiment
[0039] Example 2
[0040] Figure 1a It is the change of fluorescence spectrum of hypochlorous acid fluorescent probe (5μM) added to hypochlorous acid (0-5μM). Figure 1b It is a linear relationship graph of different concentrations of hypochlorous acid (0-1μM) versus probe (5μM).
[0041] Configure multiple parallel samples with a probe concentration of 5 μM in a 10 mL colorimetric tube, then add hypochlorous acid of different concentrations to the test system, shake it evenly and let it stand for 2 minutes. The above measurement was carried out in pure water (5mM PBS, pH 7.4), the probe used was the probe prepared in Example 1, and all the spectral measurements were measured at 25°C.
[0042] Use a fluorescence spectrometer to test its fluorescence intensity change, from Figure 1a It can be clearly seen that as the concentration of hypochlorous acid increases, the fluorescence intensity at 557nm gradually increases. And, by inserting Figure 1b It can be seen that at 557nm, the flu...
Example Embodiment
[0043] Example 3
[0044] figure 2 It is the response time of probe (5μM) after adding hypochlorous acid (5μm). Take 50μL from the probe mother liquor and place it in a 10mL test system, and then add 5μM hypochlorous acid to the test system. After shaking it evenly, use a fluorescence spectrometer to test its fluorescence intensity change immediately. The above measurement was carried out in pure water (5mM PBS, pH 7.4), the probe used was the probe prepared in Example 1, and all the spectral measurements were measured at 25°C.
[0045] It can be clearly seen from the figure that when hypochlorous acid is added, the fluorescence intensity reaches the maximum value after detection for about 2 minutes and remains unchanged, which indicates that the probe reacts quickly with hypochlorous acid and can provide rapid determination of hypochlorous acid. Analysis method.
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