Urine samples were collected from seven farmers before and after applying 20% amitraz EC to pear and citrus fields. Amitraz and its metabolites including BTS-27919, BTS-27271, and 2,4-dimethylaniline were eluted with n-hexane, dichloromethane and methanol in sequence from SPE-C18 cartridge by loading 5 mL of urine before GC-MSD determination. The mean recoveries of amitraz, BTS- 27919, BTS-27271 and 2,4-dimethylaniline were 75.7 ± 4.2 , 81.3 ± 2.4 , 87.7 ± 3.7 and 83.3 ± 1.8%, respectively. Neither amitraz nor metabolites were detected in any of the seven farmers’ urine samples.