Abstract: The soil sample was extracted with the mixture of acetone and n-hexane (volume ratio of 1∶2). After purification with PSA/Silica composite packing glass column, the eluent was collected, and then evaporated to near dryness by rotary. After adding n-hexane, GC-MS/MS was applied to the determination of 16 phthalate esters (PAEs) in the diluent. The DB-5MS quartz capillary chromatographic column was used for GC separation and the selected ion monitoring mode was adopted in MS/MS determination. For determination of 2 monoester metabolites of phthalate esters (MPEs), the eluent was evaporated to near dryness by rotary,and then derivatized for 30 min with mixture of boron trifluoride (14%, mass fraction) and methanol at 60 ℃. Linearity ranges of the 16 PAEs were found in the same range of 0.02-0.80 mg·L^-1 with detection limits (3S/N) of 1.357 μg·kg^-1. Linearity ranges of the 2 MPEs were found in the same range of 0.05-1.00 mg·L^-1 with detection limits (3S/N) in the range of 0.217 μg·kg^-1. On the base of blank soil sample, test for recovery was made by standard addition method; values of recovery found were in the range of 71.1%-105%, with RSDs (n=5) of determined values in the range of 0.10%-14%.