Abstract: Thousands of vegetable samples were tested for the multi-residue analysis of organophosphorus pesticides in vegetables according to Chinese method NY/T761-2004, the final identification of organophosphorus pesticides in vegetables was made by GC/MS, and the matrix interference with the multi-residue analysis of organophosphorus pesticides in vegetables was evaluated. There was almost no matrix interference with the multi-residue analysis of organophosphorus pesticides in leafy greens, Chinese cabbage, gourd, solanaceous fruits, legume, tuber taro and root crop vegetables. There was some matrix interference with the multi-residue analysis of organophosphorus pesticides in cabbage vegetables and the analysis of dichlorovos, methamidophas, phorate and chlorpyrifos-methyl in purple cabbage, cabbage and broccoli was usually interfered with, and there was so serious matrix interference with organophosphorus pesticides in alliaceous vegetables(e.g., garlic, shallot and leek) that the multi-residue analysis of organophosphorus pesticides in alliaceous vegetables could not be done according to Chinese method NY/T761-2004.