In this research, a straightforward sample treatment for multiresidue pesticide evaluation of onion samples was developed using the solid-phase extraction/quick, easy, cheap, effective, rugged, and secure (SPE/QuEChERS) method. The suggested technique is based on acetonitrile liquid-liquid partitioning, then follows dispersive solid-phase extraction with ZrO2 particles for extract purification. ZrO2 is synthesized via co precipitation and analyzed via XRD, FTIR, and SEM. ZrO2 has been demonstrated to be more effective than normal graphitized carbon black at eliminating pigment. Thirty-five pesticides from various chemical classes were examined using gas chromatography and tandem mass spectrometry (GC-MS/MS) to assess the outlined technique. Most analytes had recoveries in the range of 74–105%, with relative standard deviations of less than 14%. The linearity, precision, and accuracy of GC-MS/MS were adequate. The validated technique was applied effectively to onion samples from the farmer’s field.