Determination of phthalate esters residue in aquatic products by solid phase extraction with gas chromatography-mass spectrometry

A method was developed for the determination of 6 common phthalate esters(PAEs) in aquatic products by gas chromatography-mass spectrometry(GC-MS). The PAEs were extracted by cyclohexane-ethyl acetate(1:1) mixed solution, degreased by acetonitrile saturated n-hexane, then extracted by N-hexane saturation of acetonitrile, and purified by PAE30006-C SPE glass column, washed by 1% ethyl acetate and eluted by hexane-ethyl acetate(1:1), the eluent was concentrated and dissolved in hexane, and analyzed by GC-MS. The results were showed that: the linear range of 6 PAEs were 10～5000 ng/mL, and the correlation coefficients were 0.9992～0.9998, limits of detection(LOD) were 0.62～2.96 μg/kg, limits of quantifications(LOQ )were 2.0～9.0 μg/kg, The average recovery of the added test in tilapia from 10,50,100 μg/kg was 70.5%～105.4%，and the relative standard deviations(RSD) was 3.78%～7.57%. The average recovery of the added test with 50 ug/kg in Pacific white shrimp, grass carp, mud crab, yellow croaker and oyster was 71.5%～102.5%, and the RSD was 3.25%～7.86%. The method was suitable for the determination of PAEs in aquatic products with high extraction efficiency and purification effect.