A simple method for the spectrophotometric determination of cephalosporins in pharmaceuticals using variamine blue

A simple spectrophotometric method for the determination of cefotaxime, ceftriaxone, cefadroxil and cephalexin with variamine blue is presented. The determination is based on the hydrolysis of β-lactam ring of cephalosporins with sodium hydroxide which subsequently reacts with iodate to liberate iodine in acidic medium. The liberated iodine oxidizes variamine blue to violet colored species of maximum absorption at 556 nm. The absorbance is measured within the pH range of 4.0-4.2. Beer's law is obeyed in the range of 0.5-5.8 µg mL-1, 0.2-7.0 µg mL-1, 0.2-5.0 µg mL-1 and 0.5-8.5 µg mL-1 for cefotaxime, ceftriaxone, cefadroxil and cephalexin respectively. The analytical parameters were optimized and the method is successfully applied for the determination of cefotaxime, ceftriaxone, cefadroxil and cephalexin in pharmaceuticals.

A simple spectrophotometric method for the determination of methyldopa using p-chloranil in the presence of hydrogen peroxide

A simple, rapid and sensitive spectrophotometric method has been developed for the determination of methyldopa in pharmaceutical formulations. The method is based on the reaction between tetrachloro-p-benzoquinone (p-chloranil) and methyldopa, accelerated by hydrogen peroxide (H2O2), producing a violet-red compound (λmax = 535 nm) at ambient temperature (25.0 ± 0.2 ºC). Experimental design methodologies were used to optimize the measurement conditions. Beer's law is obeyed in a concentration range from 2.10 x 10-4 to 2.48 x 10-3 mol L-1 (r = 0.9997). The limit of detection was 7.55 x 10-6 mol L-1 and the limit of quantification was 2.52 x 10-5 mol L-1. The intraday precision and interday precision were studied for 10 replicate analyses of 1.59 x 10-3 mol L-1 methyldopa solution and the respective coefficients of variation were 0.7 and 1.1 %. The proposed method was successfully applied to the determination of methyldopa in commercial brands of pharmaceuticals. No interferences were observed from the common excipients in the formulations. The results obtained by the proposed method were favorably compared with those given by the Brazilian Pharmacopoeia procedure at 95 % confidence level.

A novel indicator reaction for the catalytic determination of V(V) at ppb levels by the kinetic spectrophotometric method

A novel sensitive and relatively selective kinetic method is presented for the determination of V(V), based on its catalytic effect on the oxidation reaction of Ponceau Xylydine by potassium bromate in presence of 5-sulfosalicylic acid (SSA) as activator. The reaction was monitored spectrophotometrically by measuring the decrease in absorbance of Ponceau Xylydine at 640 nm between 0.5 to 7 min (the fixed time method) in H3PO4 medium at 25ºC. The effect of various parameters such as concentrations of H3PO4, SSA, bromate and Ponceau Xylydine, temperature and ionic strength on the rate of net reaction were studied. The method is free from most interferences, especially from large amounts of V(IV). The decrease in absorbance is proportional to the concentration of V(V) over the entire concentration range tested (1-15 ng mL−1) with a detection limit of 0.46 ng mL-1 (according to statistical 3Sblank/k criterion) and a coefficient of variation (CV) of 1.8% (for ten replicate measurement at 95% confidence level). The proposed method suffers few interferences such as Cr(VI) and Hg(II) ions. The method was successfully applied to the determination of V(V) in tap water, drinking water, bottled mineral water samples and a certified standard reference material such as SRM-1640 with satisfactory results. The vanadium contents of water samples were also determined by FAAS for a comparison. The recovery of spiked vanadium(V) was found to be quantitative and the reproducibility was satisfactory. It was observed that the results of the SRM 1640 were in good agreement with the certified value.

Determination of patulin in apple juice by HPLC using a simple and fast sample preparation method

The goal of this work was to develop a simple and rapid preparation method for patulin analysis in apple juice without previous clean-up. This method combined sonication and liquid extraction techniques and was used for determination of patulin in 37 commercial apple juices available on the market in the South of Brazil. The method performance characteristics were determined using a sample obtained in a local market fortified at five concentration levels of patulin and done in triplicates. The coefficient of variation for repeatability at the fortification level of 20.70µg.L-1 was 3.53 % and the recovery 94.63 %, respectively. The correlation coefficient was 0.9996 and agrees with the requirements for a linear analytical method value. The detection limit was 0.21µg.L-1 and the quantification limit 0.70 µg.L-1. Only three of the analyzed samples were upper the allowed level of 50.00 µg.L-1 recommended for the World Health Organization.