Determination of total phthalates in edible oils by high-performance liquid chromatography coupled with photodiode array detection

Abstract

The previously reported procedure for the determination of the total phthalate in fatty food involved the extraction of phthalates using chloroform/methanol followed by the removal of the solvents before alkaline hydrolysis requiring 20 h and derivatization of phthalic acid. In this study, a phase-transfer catalyst (tetrabutylammonium chloride) was used in the liquid-liquid heterogeneous hydrolysis of phthalates in oil matrix shortening the reaction time to within 25 min. The resulting phthalic acid in the hydrolysate was extracted by a novel molecular complex based dispersive liquid-liquid microextraction method coupled with back-extraction before high-performance liquid chromatography coupled with photodiode array detection. Under the optimal experimental conditions, the linearity of the method was in the range of 0.5-12 nmol/g with the correlation coefficients (r) >0.997. The detection limit (S/N = 3) was 0.11 nmol/g. Intraday and interday repeatability values expressed as relative standard deviation were 3.9 and 7.1%, respectively. The recovery rates ranged from 82.4 to 99.0%. The developed method was successfully applied for the analysis of total phthalate in seven edible oils.