Use of capillary electrophoresis in the characterization of sulfonated metallophthalocyanines: a comparative evaluation of purification procedures following synthesis by the condensation method.

摘要: Capillary electrophoresis has been presented as a resourceful technique for monitoring the purity of synthetic metallophthalocyanines and evaluating comparatively purification procedures. In this study, tetrasulfonated cobalt(II) phthalocyanine was synthesized by condensation method submitted to several procedures such continuous Soxhlet extraction with ethanol dioxane, percolation through gel-filled chromatographic column, salting-out precipitation in acid medium followed washing alkaline solution. The efficiency each procedure, or combined procedures, then evaluated capillary citrate buffer solution under constant voltage conditions direct UV-VIS detection at 630 nm 260 nm. inorganic anion cation composition purified fractions also investigated indirect UV analysis chromate/cetyltrimethylammonium bromide (CTAB) imidazole/hydroxyisobutyric (HIBA) electrolyte systems, 254 214 nm, respectively. electropherograms obtained showed high-intensity peak surrounded satellite peaks small intensity migration time approximately 5-6 min. This profile is indicative formation positional isomers synthesis conditions. were useful monitor contaminants, reaction by-products unreacted starting materials. crude product led good-quality 80% (elemental based on nitrogen content), which comparable commercially available derivatives. Both infrared (IR) spectra resemble that standards. ion treated revealed presence sodium carbonate major contaminant. treatment Sephadex column (Pharmacia, Sao Paulo, Brazil) successful removal ion. However, procedure seemed cause minor demetallation macrocycle ring, confirmed free electropherogram eluted fraction.