Study and voltammetric determination of fipronil in bovine lactose-free milk by differential pulse voltammetry using a carbon paste electrode

A novel voltammetric screening method has been developed for the rapid determination of fipronil (FPN) residues in lactose-free milk samples with the use of a carbon-paste electrode (CPE) by differential-pulse voltammetry (DPV). Cyclic voltammetry indicated the occurrence of an irreversible anodic process at approximately +0.700 V (vs. Ag|AgCl, 3.0 mol L-1 KCl) in a 0.100 mol L-1 NaOH supporting electrolyte prepared as a 30% (v/v) ethanol-water solution. Quantification of FPN was carried out by DPV and analytical curves were constructed. In the absence of a matrix, the limits of detection (LOD) and quantification (LOQ) were 0.568 mg L-1 and 1.89 mg L-1, respectively. In the presence of a lactose-free skim milk matrix, the values of LOD and LOQ were 0.331 mg L-1 and 1.10 mg L-1. The recovery percentages for three different concentrations of FPN in lactose-free skim milk samples ranged between 95.3% and 109%. All assays could be conducted with milk samples without any prior extraction steps or pre-concentration of FPN, making this novel method rapid, simple, and relatively cheap.

Automated summary

A novel voltammetric screening method using a carbon-paste electrode (CPE) and differential-pulse voltammetry (DPV) was developed for the rapid determination of fipronil (FPN) residues in lactose-free milk samples. Cyclic voltammetry revealed an irreversible anodic process at approximately +0.700 V (vs. Ag|AgCl, 3.0 mol L-1 KCl) in a 0.100 mol L-1 NaOH supporting electrolyte prepared as a 30% (v/v) ethanol-water solution. The method allowed for the quantification of FPN in milk samples without prior extraction steps or pre-concentration of FPN, with limits of detection (LOD) ranging from 0.568 to 0.331 mg L-1 and limits of quantification (LOQ) ranging from 1.89 to 1.10 mg L-1.