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  • Title: Determination of phthalate esters in edible oils by use of QuEChERS coupled with ionic-liquid-based dispersive liquid-liquid microextraction before high-performance liquid chromatography.
    Author: Xie Q, Liu S, Fan Y, Sun J, Zhang X.
    Journal: Anal Bioanal Chem; 2014 Jul; 406(18):4563-9. PubMed ID: 24817350.
    Abstract:
    A selective and low organic-solvent-consuming method of sample preparation combined with high-performance liquid chromatography with diode-array detection is introduced for analysis of phthalic acid esters in edible oils. Sample treatment involves initial liquid-liquid partitioning with acetonitrile, then QuEChERS cleanup by dispersive solid-phase extraction with primary secondary amine as sorbent. Preconcentration of the analytes is performed by ionic-liquid-based dispersive liquid-liquid microextraction, with the cleaned-up extract as disperser solvent and 1-hexyl-3-methylimidazolium hexafluorophosphate as extraction solvent. Under the optimized conditions, correlation coefficients (r) were 0.998-0.999 and standard errors (S y/x ) were 2.67-3.37 × 10(3) for calibration curves in the range 50-1000 ng g(-1). Detection limits, at a signal-to-noise ratio of 3, ranged from 6 to 9 ng g(-1). Intra-day and inter-day repeatability, expressed as relative standard deviation, were in the ranges 1.0-6.9 % and 2.4-9.4 %, respectively. Recovery varied between 84 % and 106 %. The developed method was successfully used for analysis of the analytes in 28 edible oils. The dibutyl phthalate content of four of the 28 samples (14 %) exceeded the specific migration limit established by domestic and international regulations.
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