Bisdansylhistidine and its application
A bisdansyl histidine and solution technology, applied in the field of the new compound bisdansyl histidine, can solve the problems of difficult detection of metal ions, difficulty in real-time detection, poor water solubility of probes, etc. Achieve the effect of good water solubility, high accuracy and high sensitivity
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Embodiment 1
[0038] Embodiment 1: the synthesis of bisdansyl histidine
[0039] The synthetic route of bis dansyl histidine is as follows:
[0040]
[0041] 1) Add 0.1245g histidine (0.65mmol) into a round bottom flask, take 15.0ml of sodium bicarbonate solution with a concentration of 0.10mol / L to dissolve it, and put it in an ice-salt bath to cool for 10min;
[0042] 2) Dissolve 0.035g of dansyl chloride (0.13mmol) in 5.0mL of acetonitrile, and add the solution of dansyl in acetonitrile to the above histidine solution dropwise with a separatory funnel, and stir the solution while adding. The reaction system was stirred and reacted in the ice-salt bath for 30 minutes, then withdrawn from the ice-salt bath, and continued to react at room temperature for 3 hours. During the reaction, the reaction progress was monitored by thin layer chromatography (TLC) until the reaction was completed. ;
[0043] 3) The reaction mixture was distilled out of acetonitrile by vacuum distillation, and t...
Embodiment 2
[0046] Embodiment 2: iron ion concentration detection method
[0047] (1) Effect of pH value on recognition of iron ions by bisdansylhistidine
[0048] Add bisdansyl histidine to aqueous solutions with different pH values, and configure different pH values but the concentration is 2.0×10 -6 mol / L bisdansyl histidine solution, record the fluorescence intensity values respectively, and then add an equal amount of FeCl 3 solution, making Fe 3+ 2.0×10 -5 mol / L, calculated by adding Fe 3+ After the difference of fluorescence intensity (excitation wavelength is 330nm, emission wavelength is 501nm), and draw a graph, such as image 3 as shown, image 3 Add Fe for bisdansylhistidine at pH from 2.5 to 10.35 3+ Change value of fluorescence intensity before and after, where I 0 Represents no Fe 3+ The fluorescence intensity value of bisdansylhistidine under the excitation wave (330nm) in the presence of I represents the presence of Fe 3+ Fluorescence intensity values of ...
Embodiment 3
[0065] Example 3: Fluorescence recovery of bisdansylhistidine
[0066] After continuous experimental exploration, it was found that bisdansyl histidine and Fe 3+ After adding a certain amount of sodium phosphate to the system after the action, the fluorescence intensity of bisdansyl histidine can be recovered to a large extent, such as Figure 9 , where a represents the fluorescence spectrum of the bisdansyl histidine solution, and b represents the addition of FeCl to a3 solution, making Fe 3+ The concentration is 2.0×10 -5 mol / L fluorescence spectrum, c represents adding 1.0×10 -4 Fluorescence spectrum after mol / L sodium phosphate.
[0067] From Figure 9 It can be seen that when adding Fe 3+ When sodium phosphate is added to 5 times the amount (the multiple of the amount of the substance), the fluorescence intensity of the dansylhistidine solution can basically return to the initial state. This shows that dansylhistidine is Fe 3+ The fluorescent probes have good rev...
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