Abstract:To simultaneously determine residues of five herbicides, namely MCPA,2,4,5–T, haloxyfop–p–methyl, quizafop–p–ethyl and fluazifop–p–butyl in paddy soil, water and coarse rice, a new method was developed using high performance liquid chromatography . The residues in soil was extracted with mixed solution of 0.05% ortho-phosphoric acid and aetonitrile (volume ratio of 1∶2), and those in water was extracted with ethyl acetate , while in coarse rice was dissolved by 0.04 mol/L sodium hydroxide aqueous, then purified by a florisil column. Five herbicides were detected at uv wavelength of 229 nm with acetonitrile-water (pH=3) as mobile phase through gradient elution in HPLC, external standard was adopted as the quantification method. The linearity was good (r>0.999 7) in concentration range of 0.05 to 5.00 mg/L .Mean recoveries of five herbicides in soil and coarse rice were between 78.8% and 107.8% (RSD≤7.5, n=5) at fortification levels of 0.05 to 1.00 mg/kg, while they were between 86.2% and 109.2%(RSD≤6.5, n=5)in water at levels from 0.01 to 0.50 mg/kg. Under these optimal condition, The limit of detection for the five ingredients were between 0.01 to 0.02 mg/kg, and the limit of quantification in soil, coarse rice and water were 0.05 mg/kg, 0.05 mg/kg, and 0.01 mg/L respectively. Pre-treatment process of the method was simple, and sensitivity and accuracy of the method meet the technical requirement for the analysis and detection of pesticide residues.