Iridium complex as well as preparation method and application thereof to detection of sulfur dioxide
A technology of complexes and reactions, which is applied in the field of preparation of cyclometalated iridium complexes, can solve the problems of low sensor sensitivity, inability to directly apply detection, inability to detect sensitivity, etc., and achieve high dyeing sensitivity, weak background fluorescence intensity, cell The effect of strong penetration
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Embodiment 1
[0024] (1) 2,2'-bipyridine-N-oxide
[0025] You can refer to the literature ( Chem. Comm. 2011, 47 , 11011-11013) method to prepare. Dissolve 7.8 g of 2,2’-bipyridine in 40 mL of trifluoroacetic acid, add 8.5 mL of 30% hydrogen peroxide, stir at room temperature for 4 h, neutralize with 6N sodium hydroxide solution, and then use 4′ 50 cm 3 After extraction with chloroform, the organic phases were combined and washed with saturated sodium chloride solution, then dried over anhydrous sodium sulfate, filtered, and evaporated to remove chloroform to obtain a colorless oil, which was dried in vacuo overnight to obtain a white needle-like solid.
[0026] (2) 4-Nitro-2,2'-bipyridine-N-oxide
[0027]Dissolve 3 g of 2,2'-bipyridine-N-oxygen in 19 mL of concentrated sulfuric acid with stirring in an ice bath, then add dropwise to the mixed acid of fuming nitric acid / concentrated sulfuric acid (30 mL / 14 mL) for 15 min After completion, the temperature was raised to 100 °C and reflu...
Embodiment 2
[0036] Example 2 [Ir(ppy) 2 azobpy Ir(ppy) 2 ] 2+ to SO 2 in vitro response experiment
[0037] The complexes used below are the compounds prepared in Example 1.
[0038] Prepare a 10 mM complex solution with acetonitrile / HEPES (10 mM, pH 7.5) buffer solution with a volume ratio of 1:1, add sodium sulfite solutions of different concentrations dropwise, stir well, let stand at room temperature for 5 min, and then measure the UV absorption spectrum and fluorescence intensity. The excitation wavelength and maximum emission wavelength of the complex are 400 and 560 nm, respectively. The experimental results are image 3 , Figure 4 . Depend on image 3 It can be seen that after adding a small amount of sodium sulfite solution, the ultraviolet absorption spectrum of the complex changes significantly, the absorption near 280 nm is enhanced, and the absorption near 400 nm is weakened, indicating that the complex can combine with solution-type SO 2 (sodium sulfite) reacte...
Embodiment 3
[0039] Example 3 [Ir(ppy) 2 azobpy Ir(ppy) 2 ] 2+ to SO 2 Intracellular response experiments
[0040] The complexes used below are the compounds prepared in Example 1.
[0041] Cell culture: Hela cells were cultured in DMEM medium containing 10% fetal bovine serum, cells (5′ l0 8 / L) inoculated in a confocal microscope special glass-bottom culture dish, the diameter of the culture dish is 35 mm, the thickness of the cover glass is 0.085~0.13 mm, the diameter of the micropore in the center of the dish is 10 mm, and 5% CO 2 Incubate at 37°C under 95% air conditions, and after 24 hours of adherent growth, replace with serum-free medium and continue to incubate for 4 hours.
[0042] Confocal microscope-cell imaging: Hela cells were first incubated with different concentrations of sodium sulfite solution for 1 hour, then the medium was aspirated, replaced with PBS, and the complex (5 μM) was added to continue to incubate for 30 minutes, then the PBS was aspirated, and then w...
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