Generation and destruction of unstable reagent in flow injection system: determination of acetylcysteine in pharmaceutical formulations using bromine as reagent.

A flow injection spectrophotometric procedure was developed for determination of acetylcysteine in sachets and liquid formulations. The determination of this drug was carried out by reacting it with bromine chemically generated in flow injection system monitored continuously at 400 nm. Acetylcysteine reacts with bromine causing a decrease in the absorbance that is proportional to the analyte concentration. The bromine in excess was destroyed on-line by an ascorbic acid solution before the discard. The calibration curve for acetylcysteine determination was linear in the concentration range from 1.6 x 10(-4) to 1.6 x 10(-3) mol/l with a detection limit of 8.0 x 10(-5) mol/l. The relative standard deviation (R.S.D.) was lesser than 1.2% for a solution containing 5.3 x 10(-4) mol/l acetylcysteine (n=10), and 60 determinations per hour were obtained.

Electroregenerable anion-exchange resin with triiodide carbon paste electrode for the voltammetric determination of adrenaline.

An electroregenerable carbon paste electrode modified with triiodide ions immobilized in an anion-exchange resin (Lewatit M500) is proposed for the determination of adrenaline in pharmaceutical products by differential-pulse voltammetry (DPV). Adrenaline was chemically converted into adrenochrome by the I3- ions at the electrode surface. The electrochemical reduction back to adrenaline was obtained at a potential of -0.16 V vs. Ag/AgCl (3 mol l(-1) KCl). A 20% decrease of the initial analytical signal was observed after 350-400 determinations; the carbon paste electrode was 100% electroregenerated at a fixed potential of +0.65 V vs. Ag/AgCl (3 mol l(-1) KCl) in 0.1 mol l(-1) KI solution for 20 min. The differential-pulse voltammograms were obtained by applying a sweep potential between 0.0 and -0.34 V, following the adrenochrome reduction at -0.16 V. Under the optimum conditions established, such as pH 6.0; scan rate 20 mV s(-1) and pulse amplitude 50 mV, the calibration curve was linear from 2.0 x 10(-5) to 3.1 x 10(-4) mol l(-1) adrenaline with a detection limit of 3.9 x 10(-6) mol l(-1). The recovery of adrenaline ranged from 99.8 to 103.1% and the RSD was 2.6% for the solution containing 1.0 x 10(-4) mol l(-1) adrenaline (n = 10). The results obtained for adrenaline in pharmaceutical samples using the proposed carbon paste electrode are in agreement with those obtained using a pharmacopoeial procedure at the 95% confidence level.