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Determination of 16 phthalate esters in sesame oil by isotope dilution liquid chromatography with tandem mass spectrometry

Abstract

Phthalate esters are easily released from packing materials into fat-rich food results in contamination in edible oil. This work focuses on the major aspects concerning the accurate and precise quantification of 16 phthalate esters in edible oil by isotope dilution liquid chromatography - tandem mass spectrometry, which will be helpful in the determination of true value of phthalate esters in metrological view. Oil samples were exacted by acetonitrile and n-hexane then cleaned-up by PSA SPE cartridge. Critical isomers were well separated on ZORBAX SB-Phenyl column under gradient elution followed by positive ESI-MS/MS mode. The approaches taken to optimize sample handling, solvent, and LC system helped to reduce the blank interferences, and thereby improved the LOD of DBP, DEHP, DEP and BBP by 50%. Quantification was based on the measurement of mass ratios of the natural and corresponding D4 isotopically labeled internal standards in the sample by using a single-point calibration. The spiking recoveries of 16 analytes ranged from 88.6 to 105.6% with relative standard deviation values between 0.3 and 7.5%. The detection limits for 16 analytes were 0.21 - 28.2 ng/g. The relative expanded uncertainties were from 4.2 to 15%. Together with the decrease of blank interference, superior selectivity for the isomeric mixtures and use of isotopically labeled internal standards, the method was confirmed to be a reference method to provide an accuracy base to determine trace phthalate esters in edible oil.

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Publication details

The article was received on 26 Feb 2018, accepted on 26 May 2018 and first published on 29 May 2018


Article type: Paper
DOI: 10.1039/C8AY00422F
Citation: Anal. Methods, 2018, Accepted Manuscript
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    Determination of 16 phthalate esters in sesame oil by isotope dilution liquid chromatography with tandem mass spectrometry

    X. Li, Q. H. Zhang, L. Chen, J. Zhao and H. Li, Anal. Methods, 2018, Accepted Manuscript , DOI: 10.1039/C8AY00422F

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