The water soluble 5-paminophenyl)-10,15,20-tris(psulfonatophenyl) porphyrin, 4, acts as an extremely efficient chromogenic reagent for the detection of very low amounts of nitriles. The amino group of porphyrin 4 reacts smoothly with nitrite in acidic conditions 0.2 M HCl) producing the corresponding diazo-porphyrin derivative which is stable and does not show any appreciable hydrolysis to phenol within 6 h. The reaction is carried out in the presence of 25 mM heptakis-(2,6-di-O-methyl)-beta-cyclodextrin that prevents precipitation of the protonated form of porphyrins 4 or 5 due to the formation of strong inclusion complexes. The capillary zone electrophoresis of the diazoporphyrin and amino-porphyrin mixture shows severe peak tailing. However, symmetrical peaks can be obtained by adding 5 mM beta-cyclodextrin to the background electrolyte (20 mM phosphate buffer, pH 7.0). Calibration curve for nitrite analysis is linear up to 0.25 mM nitrite and the detection limit (at a signal-to-noise ratio of 3) has been estimated to be a 1 mu M (50 ppb) of nitrite concentration in aqueous solutions.
A highly sensitive method for the analysis of nitrite ions by capillary zone electrophoresis using water-soluble aminophenylporphyrin derivative as chromogenic reagent.
CAROFIGLIO, TOMMASO;FORNASIER, ROBERTO;TONELLATO, UMBERTO
2000
Abstract
The water soluble 5-paminophenyl)-10,15,20-tris(psulfonatophenyl) porphyrin, 4, acts as an extremely efficient chromogenic reagent for the detection of very low amounts of nitriles. The amino group of porphyrin 4 reacts smoothly with nitrite in acidic conditions 0.2 M HCl) producing the corresponding diazo-porphyrin derivative which is stable and does not show any appreciable hydrolysis to phenol within 6 h. The reaction is carried out in the presence of 25 mM heptakis-(2,6-di-O-methyl)-beta-cyclodextrin that prevents precipitation of the protonated form of porphyrins 4 or 5 due to the formation of strong inclusion complexes. The capillary zone electrophoresis of the diazoporphyrin and amino-porphyrin mixture shows severe peak tailing. However, symmetrical peaks can be obtained by adding 5 mM beta-cyclodextrin to the background electrolyte (20 mM phosphate buffer, pH 7.0). Calibration curve for nitrite analysis is linear up to 0.25 mM nitrite and the detection limit (at a signal-to-noise ratio of 3) has been estimated to be a 1 mu M (50 ppb) of nitrite concentration in aqueous solutions.Pubblicazioni consigliate
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