A new method of high performance liquid chromatography-fluorescence detection（HPLC-FLD） was developed for the detection of 2-methylisoborneol（2-MIB）,geosmin（GSM） and 3-methyl-1-butanol（3-MB）,with 6-carbonyl chloride levofloxacin（LFC-Cl） as derivatization reagent and magnetic graphene oxide（MGO） as magnetic dispersive solid phase extraction（MDSPE） adsorbent.Through optimizing derivatization conditions,three kinds of volatile organic compounds（VOCs） could be completely derivatized in 0.05 mol/L 4 dimethylaminopyridine（DMAP）acetonitrile solution within 90 min at 60 ℃ under ultrasonic assisted conditions.Through optimizing MDSPE conditions,three VOCs derivatives could be enriched and purified by a 20 min extraction of 20 mg adsorbent followed by a 3 min desorption of acetonitrile containing 1% formic acid.Under the optimized chromatographic conditions,the baseline separation and high sensitive detection of three VOCs derivatives were realized within 15 min.The limits of detection（LOD） and limits of quantitation（LOQ） of this method were in the ranges of 0.020-0.95 ng/L and 0.10-3.3 ng/L,respectively.The linearity,precision and recoveries were satisfactory.Compared with the reported methods,this method had the advantages of high sensitivity,simple sample pretreatment and universal instruments.It was suitable for the rapid determination of three VOCs in pond water and vegetables,providing a new approach for the monitoring of food and environmental water samples.