Iridium complex containing (aldehyde) phenanthroline ligand and method for quantitatively detecting bisulfite by using iridium complex containing (aldehyde) phenanthroline ligand
A technology of bisulfite and iridium complexes, applied in the field of fluorescent materials, to achieve good selectivity, high sensitivity, and good stability
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[0041] (1) Preparation of chlorine-bridged dimers
[0042] Under nitrogen protection, 0.3528g (1mmol) of IrCl 3 ·3H 2 O was added to the mixed solvent of 2-ethoxyethanol and water, 2-ethoxyethanol: water (V:V) = 30:10mL, magnetically stirred for 15min, after stirring evenly, 321μL (2.2mmol) of 2-Phenylpyridine, heated to 120°C, refluxed, stirred for 24 hours, then stopped the reaction, cooled to room temperature, and filtered with suction to obtain a precipitate, which was washed with 30mL secondary deionized water, 30mL ethanol and 30mL n-hexane, respectively, at 50°C Vacuum baked in a drying oven for 12 hours to dryness to obtain orange-red powdery chlorine-bridged dimer;
[0043] (2) Synthesis of iridium complexes
[0044] Under the protection of nitrogen, 0.11g (0.1mmol) of chlorine bridge dimer and 0.048g (0.228mmol) of 5-formyl-1,10phenanthroline were mixed according to the molar ratio of 1:2.28 and added to 50mL of dichloromethane In the solvent, heat to 40°C, stir ...
Embodiment 1
[0048] In this embodiment, the above-mentioned iridium complex (abbreviation: iridium complex) containing (aldehyde group) phenanthroline ligand is used as a fluorescent probe to detect the bisulfite content in the sample to be tested, and the specific detection method is realized by the following steps :
[0049] (1) Preparation pH is 5.0, concentration is the acetic acid-sodium acetate buffer solution of 10mmol / L, then prepare the dimethyl sulfoxide solution of the iridium complex with concentration of 1mmol / L and the standard hydrogen sulfite radical of 1mmol / L aqueous solution;
[0050] (2) In a 10mL centrifuge tube, add 5mL acetic acid-sodium acetate buffer solution with a pH of 5.0 and a concentration of 10mmol / L and 300μL of a dimethyl sulfoxide solution of a 1mmol / L iridium complex in sequence, and then add 0, 4, 10, 20, 30, 40, 50, 60, 70, 80, 90μL standard bisulfite aqueous solution with a concentration of 1mmol / L, and then add a certain volume of acetic acid-sodium...
Embodiment 2
[0057] The present embodiment uses the above-mentioned iridium complex containing (aldehyde group) phenanthroline ligand as a fluorescent probe to detect the bisulfite content in the sample to be tested, and the specific detection method is realized by the following steps:
[0058] (1) The disodium hydrogen phosphate-citric acid buffer solution with a pH of 3.0 and a concentration of 10mmol / L is prepared, and then the dimethyl sulfoxide solution of the iridium complex with a concentration of 1mmol / L and the standard sulfoxide solution with a concentration of 1mmol / L are prepared. Hydrogen sulfate aqueous solution;
[0059] (2) In a 10mL centrifuge tube, add 5mL of dimethyl sulfoxide solution with a pH of 3.0 and a concentration of 10mmol / L disodium hydrogen phosphate-citrate buffer and 300μL of a 1mmol / L iridium complex in sequence, and then add Add 0, 4, 10, 20, 30, 40, 50, 60, 70, 80, 90 μL of standard bisulfite aqueous solution with a concentration of 1 mmol / L, and then add...
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