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A rapid and simple method for the extraction and preconcentration of N-methylcarbamates (NMCs) (carbofuran, carbaryl and promecarb) in water samples using dispersive liquid–liquid microextraction (DLLME) using chemometrics was developed. Influence variables such as volume of extracting (CHCl₃) and dispersing solvents (ACN), pH and ionic strength, extraction time and centrifugation time and speed were screened in a 2^7–4 Plackett–Burman design was investigated. The significant variables were optimized by using a central composite design (CCD) combined with desirability function (DF). At optimum conditions values of variables set as 126 μL chloroform, 1.5 mL acetonitrile, 1 min extraction time, 10 min centrifugation at 4000 rpm min⁻¹, natural pH, 4.7% (w/v) NaCl, the separation was reached in less than 14 min using a C₁₈ column and an isocratic binary mobile phase (acetonitrile: water (50:50, v/v …