Simultaneous Determination of Nine Phthalates in Vegetable Oil by Atmospheric Pressure Gas Chromatography with Tandem Mass Spectrometry (APGC-MS/MS)

Abstract

Although the use of phthalates has been restricted worldwide, they remain an issue due to health concerns. Diet is one of the most important exposure pathways for humans and due to their solubility in oil, phthalates are commonly found in edible oil and food high in fat. Gas chromatography–mass spectrometry (GC-MS) using electron ionization (EI) has been commonly used for the analysis of the phthalates in foodstuffs, including edible oil. However, this method suffers from issues with sensitivity and selectivity, as most phthalates are fragmented to generate a common phthalic anhydride fragment ion at m/z 149. The molecular ion cannot be observed due to strong fragmentation in EI. In contrast, atmospheric pressure gas chromatography (APGC) is a soft ionization technique with less fragmentation, whereby the molecular ion can be used as the precursor ion for multiple reaction monitoring (MRM). In this study, a simple and quick method for the determination of phthalates in vegetable oil using APGC-MS/MS was developed, and performance was assessed. The method was based on dilution of the oil in solvent and direct injection without the need for further cleanup. The established method was evaluated for linearity, recovery, precision, method detection limit (MDL), and method quantitation limit (MQL). The obtained MQL in vegetable oil was in the range of 0.015–0.058 mg/kg, despite limiting the injection volume to 1 µL, which is suitable for investigating dietary exposure and future proof against decreases to the regulatory limit. Finally, the developed method was successfully applied to analyze nine phthalates in eight commercially available vegetable oil.

Unpacking Phthalates from Obscurity in the Environment

“…As a result, there is a need to develop sensitive and robust methods for extracting and determining a wide variety of PAEs. For instance, spiking methods and careful sample reconstitution are highly recommended [ 102 ]. The second challenge arises from the ubiquity of PAEs in everyday human life.…”

Development and validation of a GC Orbitrap-MS method for the analysis of phthalate esters (PAE) and bis(2-ethylhexyl)adipate (DEHA) in atmospheric particles and its application for screening PM2.5 from Curitiba, Brazil

“…This is particularly challenging when assessing data for di-isononyl phthalate (DINP) and di-isodecyl phthalate (DIDP). GC-SQ/MS analysis of DINP and DIDP results in two overlapping clusters of unresolved peaks corresponding to different branched isomers 48 which can potentially be resolved by GC-Orbitrap-MS systems.…”