The partial least squares (PLS-1) calibration model based on spectrophotometric measurement, for the simultaneous determination of sulfite and sulfide is described. This method is based on the difference between the rate of the reaction of sulfide and sulfite with Malachite Green in pH 7.0 buffer solution and at 25 ${^{circ}C}$. The absorption kinetic profiles of the solutions were monitored by measuring the decrease in the absorbance of Malachite Green at 617 nm in the time range 10-180 s after initiation of the reactions with 2 s intervals. The experimental calibration matrix for partial least squares (PLS-1) calibration was designed with 24 samples. The cross-validation method was used for selecting the number of factors. The results showed that simultaneous determination could be performed in the range 0.030-1.5 and 0.030-1.2 $mu$g m$L ^{-1}$ for sulfite and sulfide, respectively. The proposed method was successfully applied to simultaneous determination of sulfite and sulfide in water samples and whole human blood.