Abstract: Six phthalates (DBP,BBP,DEHP,DNOP,DINP and DIDP) used as plasticizers for PVC plastics for making toys were determined by hyphenated GC and MS.Samples of PVC plastics were extracted with methyl iso-butyl ketone ultrasonically.An aliquot of the extract was taken for GC-MS determination.Under the selected conditions,DBP,BBP,DEHP and DNOP were successfully separated and by comparing the data of retention time,the chromatograms and the peak area with m/z=149,qualitative and quantitative analysis were performed satisfactorily.To overcome the over-lapping of chromatograms of DINP,DIDP and DNOP,measurements of peak area of mass spectrum peaks with m/z=293 and m/z=307 were used for their determinations.Detection limits (3s) of 20 mg·kg-1 was found for DBP,BBP,DEHP and DNOP and of 100 mg·kg-1 for DINP and DIDP.Tests for recovery were made at the concentration levels of 10,20,50 mg·L-1 of the mixed phthalate standards,values of recovery found were in the range of 80%-110%.