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

Autor: Lupetti, Karina Omuro, Vieira, Iolanda Cruz, Vieira, Heberth Juliano, Fatibello-Filho, Orlando
Zdroj: Analyst; April 4, 2002, Vol. 127 Issue: 4 p525-529, 5p
Abstrakt: 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 × 10−5 to 3.1 × 10−4 mol l−1 adrenaline with a detection limit of 3.9 × 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 × 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.
Databáze: Supplemental Index