Diluted acid hydrolysate of Corn Stover was studied and identified by means of gas chromatography-mass spectrometry(GC-MS).Four mainly inhibitors were analyzed by GC-MS,including acetic acid,furfural,laevulinic acid and 5-(hydroxymethyl) furfural.The linear ranges for above four inhibitors were 0.07~0.51,0.05~0.35,0.11~0.85 and 0.08~0.63 mg/mL,respectively,with R20.995.A series of diluted acid hydrolysate of corn stover were analyzed,and it was found that the concentrations of four inhibitors were different due to the condition of hydrolysis technology,which provides an effective information to improve the hydrolysis technology.