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The need to analyze multi pesticide residues continues to be imperative and applying a suitable experimental design remains the core to achieving a comprehensive chemical analysis. The pretreatment of a sample has been found to be the most important rate-determining step as it affects the instrumental process and data analysis. The use of the SPME technique coupled with GC-MS to determine multi-residue pesticides is found to be applicable in environmental, pharmaceutical, food, clinical, forensic samples in three modes (DI-SPME, HS-SPME and MD-SPME). This has gained much recognition due to its advantage over the classical or previous sample pretreatment methods such as SPE, LLE, LDME, HFME and DLME. Before applying SPME coupled to a GC-MS detector, several conditions need to be met in order to accomplish enhanced extraction rate, efficiency and sensitivity of experimental procedures. The large numbers of data sets obtained with the advent of various instrumental techniques can be analyzed speedily by applying chemometric methods to screen the various parameters affecting the calibration methods by statistical application so as to achieve the best optimization of the experiment. This review aims at looking at the different chemometric methods for multivariate parameter optimization in experimental design for the analysis of pesticide residues in water.