Abstract: | Abstract Organophosphorus pesticides, such as parathion methyl (PTM), fenitrothion (FT), parathion (PT), and isocarbophos (ICP), have sensitive but overlapped voltammetric peaks with peak potentials ?309, ?364, ?317, and ?480 mV, respectively, in Britton‐Robinson buffer of pH 4.8 by application of linear sweep stripping voltammetry (LSSV). In this work, two multivariate calibration methods, partial least squares (both PLS‐1 and PLS‐2), and principal component regression (PCR), were applied to quantitatively resolve the overlapping voltammogram of the mixtures of these four pesticides. The prediction results obtained from a set of independent test samples showed that PLS‐1 method performed better prediction ability than PLS‐2 and PCR methods. The proposed method was successfully applied to the determination of these four pesticides in grain samples after a pre‐extraction step with a solvent of acetone. |