Fast and reliable BIA/amperometric quantification of acetylcysteine using a nanostructured double hydroxide sensor

Highlights

• A new nanomaterial was produced with Ni and Pb is more stable than Ni(OH)₂;

• Were obtained nanoparticles with only ~3 nm with great electrocatalytic activity;

• A BIA cell, with volume of just 4 mL, was built using a 3D printer;

• The miniaturization resulted in reduction of waste generation;

• In the time necessary for one chromatogram, using BIA is possible to perform 20 analysis.

Abstract

This study reports the preparation and characterization of nickel/lead hydroxide nanoparticles used to construct electrochemical sensors, which were investigated for amperometric quantification of N-acetylcysteine (NAC). The newly synthesised material presents good uniformity, with the lead (II) ions homogenously incorporated into the alpha nickel hydroxide crystal structure, confirmed by X-ray diffraction, transmission electron microscopy and X-ray photoelectron spectroscopy analyses. Films of nanoparticles (3 nm in size) were prepared on conductive fluorine-doped tin oxide-coated glass slides and used connected to a specially built batch injection analysis (BIA) cell with a capacity of only 4 mL and the electrode positioned in the bottom. To attain optimal analytical performance, the main parameters for BIA measurements (volume injected, different velocities of injection and best distance of the pipette from the electrode) were evaluated, as was the working potential, to determine the optimal conditions. Linear responses were obtained for the concentration range from 20 to 220 μmol L⁻¹, and the limits of detection (3σ/slope) and quantification (10σ/slope) were calculated as 0.23 μmol L⁻¹ and 0.70 μmol L⁻¹, respectively. The new NAC sensor does not exhibit a memory effect and has enormous potential utility in the quantitative determination of N-acetylcysteine in drugs. The results of the analysis of NAC obtained using BIA presented good concordance with those obtained by chromatography. The analytical frequency attained using BIA (120 analysis h⁻¹) compares very favourably with the one obtained using chromatography (6 analysis h⁻¹).