Objective To establish a method for the determination of six phthalates[diisobutyl phthalate(DIBP),di-n-butyl phthalate(DBP),di(2-butoxy)ethyl phthalate(DBEP),dicyclohexyl phthalate(DCHP),di(2-ethyl)hexyl phthalate(DEHP)and diisononyl phthalate(DINP)]in semi-solid food by gas chromatography-mass spectrometry(GC-MS/MS).Methods The optimization of chromatography and mass spectrometry conditions,the comparison of pretreatment extraction methods,and the selection of purification columns were carried out.The samples were extracted with an organic solvent,and the supernatant was purified by a solid phase extraction column made of ethylenediamine-N-propylsilane/silica gel(PSA/Silica)composite packing glass,and separated by a capillary column TG-5MS(30 m×0.25 mm×0.25 μm).The optimal conditions were selected by mass spectrometry full scan(SCAN)mode,and then by feature selective ion monitoring scan mode(SIM)detection,the retention time and qualitative ion fragment abundance ratio were qualitatively analyzed,and the external standard method was used for quantitative analysis.Results The separation was completed within 26.5 min.Linear range:DINP had a good linear relationship in the concentration range of 0.2～5.0 μg/mL,with r>0.9995,and the other five species had a good linear relationship in the range of 0.02～0.50 μg/mL,with>r0.9995.The limit of quantification was 9.0 mg/kg,DINP was 0.3 mg/kg,and the others were 0.5 mg/kg,and the three-level standard solution was added to the two dipping materials and bottom materials,respectively:DINP was 20,40 and 60 mg/kg,and the others were 4,6 and 8 mg/kg,and the recovery rates were 89.1%～101%.The RSD%was less than 3.8%.Conclusion This method has simple pretreatment,good selectivity,sensitivity and accuracy,and can be widely used for the determination of plasticizers in semi-solid composite seasonings.
phthalic acid eastersPAEsgas chromatography mass spectrometry
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