A dilute-and-inject low-pressure gas chromatography-tandem mass spectrometry method for phthalate determination in extra virgin olive oil

The goal of this study was to develop a method for the determination of nine phthalic acid esters in extra virgin olive oils using low-pressure gas chromatography-triple-quadrupole mass spectrometry. Sample preparation was simple, environmental friendly, and rapid inasmuch that it involved only dilution (< 1 mL of hexane). The low-pressure gas chromatography analyses were performed by using a 5 m wide-bore column. The limit of quantification for the phthalates ranged from 0.06 to 1.14 mg kg(-1). Both intra- and interday precisions were measured, with coefficient of variation values ranging from 0.2% to 11.7%. The trueness of the method was measured by evaluating accuracy at the initial stage of the work and after 2 months, with values ranging between -8.7% and 12.1%. Moreover, blind accuracy was comprised between -11.6% and 14.2%. The method involves the use of simplified instrumentation and reduced analysis times (nearly two times faster) compared to a previously published comprehensive two-dimensional gas chromatography-triple-quadrupole mass spectrometry method, leading to a reduction of energy and helium consumption. The approaches were compared in analytical terms and for the environmental impact. In total, 23 olive oil samples were analyzed, with at least one phthalate detected in all but one sample.

Automated summary

The study developed a simplified method for detecting nine phthalic acid esters in extra virgin olive oils using low-pressure gas chromatography-triple-quadrupole mass spectrometry. The method showed high precision and accuracy, with a low limit of quantification for the phthalates. Compared to a previously published method, this approach reduced energy and helium consumption and had shorter analysis times. A total of 23 olive oil samples were analyzed, with almost all samples containing at least one phthalate.