Rapid determination of phthalate esters in edible oils with short size exclusion chromatography column

Abstract

Phthalate esters are the best known of endocrine disruptors, so a simple and rapid method is proposed for the determination of eight types of phthalates [Dimethyl phthalate (DMP), Diethyl phthalate (DEP), Benzyl butyl phthalate (BBP), Dibutyl phthalate (DBP), Diisobutyl phthalate (DIBP), Diethylhexyl phthalate (DEHP), Dioctyl phthalate (DOP) and Diisodecyl phthalate (DIDP)] in edible oils. Oil samples were simply dissolved in ethyl acetate/nhexane and eight kinds of phthalates were extracted directly with size exclusion chromatography followed by gas chromatography in combination with mass spectrometry detection (GC-MS) using selected-ion monitoring (SIM). In order to develop a fast and reliable method to meet the legislations of EU, USA, etc., a variety of validation parameters and the procedures of extraction, clean up and keeping blank minimized from phthalate contamination procedure were investigated and optimized. The method detection limits varied from 0.018 mg/kg for DMP to 0.2 mg/kg for DIDP. The method observed a good repeatability results with relative standard deviation (RSD) less than 10%. The method reported an excellent accuracy confirmed with certified reference material and the overall average recovery varied between 86.8% and 95.8% at the three different levels 0.125, 0.5 and 15 mg/kg.