As a basis for the development of a sensitive analytical method for the determination of carmine food dye, a study of the differential pulse polarographic reduction of carminic acid (CA) on a dropping mercury electrode was performed. For the analytical differential pulse polarographic method running at pH 2.0 Britton-Robinson (B-R) buffer solution (peak at -489 mV), the relationship between the peak current and CA concentration was linear in the range of 1 μM to 90 μM with a detection limit of 0.16 μM. The proposed electrochemical procedure was successfully applied to the determination of carmine food dye in spiked commercially available strawberry flavored milk. The method was extended to the determination of CA in candy and results were in agreement with that obtained by a spectrophotometric comparison method. A cyclic voltammogram of CA in 2.0 B-R buffer electrolyte was obtained on the dropping mercury electrode at pH 2.0 during potential scans from 0.00 mV to 1000 mV versus Ag/AgCl. From repetitive cyclic voltammograms, one cathodic peak at -500 mV and three anodic peaks on the reverse scan between approximately -340 mV and -460 mV were recorded. The influences of some other commonly found inorganic and organic salts on the determination of CA were also examined. The sufficiently good recoveries and low standard deviations for the data reflect the high accuracy and precision of the proposed differential pulse polarographic method.
Melamine made headlines in September 2008 because it was found to be the contaminant responsible for the deaths of several infants and making many more sick. Determination of trace melamine is very important. Therefore, in this work a novel, sensitive and reliable method was developed using differential pulse polarography. The most suitable buffer system was found to be Britton-Robinson (B-R) buffer, pH 11.2. The melamine peak in this medium appeared at about −50 mV, it responded well to standard additions and high reproducibility was obtained. The calibration graph was linear in the concentration range of melamine from 1.0 to 66.4 μM with a correlation coefficient of 0.999. The limit of detection (LOD) and limit of quantification (LOQ) were obtained as 0.3 and 1.0 μM, respectively. The current was characterized as being adsorption-controlled process. The proposed method was successfully applied to the determination of melamine in spiked milk and milk powder. The linear dynamic ranges observed for melamine concentration in milk and milk powder samples were between 1-58 and 10-57 μM, respectively. The sufficiently good recoveries and low standard deviations for the data reflect the high accuracy and precision of proposed differential pulse polarographic method.
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