GC-MS Determination of Phthalates in Canned Food with Dispersive Solid Phase Extraction

Six phthalates(PAEs),namely dibutyl phthalate(DBP),benzyl-n-butyl phthalate(BBP),di-(2-ethyl hexyl)-phthalate(DEHP),di-n-octyl phthalate(DNOP),di-iso-nonyl phthalate(DINP) and di-iso-decyl phthalate(DIDP),in canned food were determined simultaneously by GC-MS under selective ion monitoring mode after separation by dispersive solid phase extraction(DSPE).Sample of canned food was extracted ultrasonically with 10.0 mL of n-hexane with 2 mL of acetonitrile as dispersion agent.The extract obtained was purified by DSPE using ethylene diamine-N-propylsilane(PSA) as solid phase material.After centrifuging,the supernatant solution was used for GC-MS analysis.Linearity ranges found were in the range of 0.1-5.0 mg·L-1 for DBP,BBP,DEHP and DNOP,and in the range of 0.5-25.0 mg·L-1 for DINP and DIDP,with correlation coefficients over 0.995.Determination limits(S/N=10) of the method obtained were 0.01 mg·kg-1 for DBP,BBP,DEHP and DNOP,and 1.0 mg·kg-1 for DINP and DIDP.Tests for recovery and precision were made by addition of standard solutions of the 6 phthalates in 3 different concentrations to canned food sample which was then analyzed by the proposed method.Values of recovery obtained were in the range of 85%-130% with values of RSD′s less than 10%.