Abstract: 25 pesticide residues including organochlorine, pyrethroid, acaricide in vegetables and fruits were determined by online GPC-GC/MS coupled with QuEChERS method. The results show that GPC of online GPC-GC/MS system can effectively remove chromatographic interferences that QuEChERS pretreating method can not effectively removed. Compared with GC/MS, online GPC-GC/MS has the lower interfered background and better peak shape. Identification and quantization of pesticide residues with online GPC-GC/MS can be well performed. All pesticides including three spiked samples (spinach, cucumber and apple) at the level of 0.01 mg/kg have 80%—120% of the recovery and less than 20% of the coefficients of variation.