Kinetic-spectrophotometric determination of Cu(II) and pyridine by use of the aerial oxidation of dimedone bisguanylhydrazone

The synthesis and analytical properties of dimedone bisguanylhydrazone (DIBG) are described for the first time. DIBG is oxidized by aerial oxygen and the reaction is catalysed by copper(II). The catalytic effect of copper(II) is increased by the presence of pyridine. Kinetic methods are described for determining trace amounts of copper(II) and pyridine. The reaction is followed spectrophotometrically by measuring the rate of change of absorbance at 550 nm. The calibration graphs are linear in the range 0.6-9.5 mug for copper(II) and 0.2-8.8 mg for pyridine. The methods have been applied to the determination of copper in galena and of pyridine in piperidine and isoamyl alcohol. The kinetic parameters of the reaction have been determined.     

Adsorptive stripping voltammetry of Tartrazine at the hanging mercury drop electrode in soft drinks

Adsorptive stripping voltammetry was used for the determination of trace amounts of the dye Tartrazine (E-102) by square-wave (SWS) and differential pulse techniques (DPS). Its adsorptive voltammetric behaviour was investigated at different pH media. NH₄Cl/NH₃ buffer solution was chosen as the most suitable, taking into account the sensitivity and definition of the reduction peaks obtained. The effects of the experimental parameters on the determination are discussed. Standard deviations of 3.3% and 2.6% were obtained by SWS and DPS for 100 and 50 μg/L Tartrazine solutions, respectively (n = 10). Both methods were applied to determine the dye in several commercial soft drinks, containing very small amounts of it. Measurements were made directly in the commercial samples. A comparison of the results obtained by the proposed voltammetric methods with those of an HPLC method was also made. Good correlations between the voltammetric results and the values supplied by the manufacturer were found, whereas recoveries of the same order of magnitude were obtained by the HPLC method. Received: 23 May 1996 / Revised: 5 July 1996 / Accepted: 10 July 1996     

Determination of sulfametoxazole, sulfadiazine and associated compounds in pharmaceutical preparations by capillary zone electrophoresis

A capillary zone electrophoresis method is presented to separate sulfadiazine, sulfamethoxazole, trimethoprim, bromhexine and guaiacol by using a fused-silica capillary (60.2 cm x 75 microm I.D.). The separation was carried out at 30 kV and 25 degrees C in a 15 mM phosphate buffer adjusted to pH 6.2 as electrolyte. Under these conditions, the run time was 6 min and the limits of quantification were about 1 mg/l for every component. The method was applied to pharmaceutical preparations and the results provided recoveries close to 100%.     

Development and validation of an analytical methodology for the determination of p,p′-DDT, p,p′-DDE and p,p′-DDD in fish oil pills

An analytical methodology was proposed and validated to be applied to the determination of p,p′-DDT and its metabolites p,p′-DDE and p,p′-DDD in fish oil. The analytical procedure presented in this paper involves a single-step clean up process prior to the analysis. A solution of 1,2,3,4-tetrachloronaphtalene was used as internal standard.The analytical technique used was gas chromatography coupled to an electron capture detector. Details on the validation process are provided.The limits of detection ranged from 2.6 to 4.7 pg μL^− 1. The BCR 598 standard reference material (cod liver oil) was used to evaluate the performance of the methodology with satisfactory recoveries for all the compounds.The analytes were determined in three different fish oil pills sold in Spain as a supplementary vitamin support. The sum of p,p′-DDT and metabolites was from 13.2 to 51.3 ng g^− 1, the dominant compound being p,p′-DDE.