Rapid and sensitive method for the determination of four EU marker polycyclic aromatic hydrocarbons in cereal-based foods using isotope-dilution GC/MS

ABSTRACT

A rapid and sensitive method has been developed for the determination of the four European Union marker polycyclic aromatic hydrocarbons (PAHs; benz[a]anthracene, chrysene, benzo[b]fluoranthene and benzo[a]pyrene) in some cereal-based foods. The method is based on pressurised liquid extraction (PLE), solid-phase extraction clean-up (SPE) and isotope-dilution gas chromatography with mass-spectrometric detection (GC/MS). The developed method was calibrated for the content range of 0.05–12.5 µg kg⁻¹ (expressed on a product basis). Recoveries of PAH were monitored in each sample via the recovery of ¹³C-labelled PAHs. Recovery values were in the range between 86% and 91%, with relative standard deviations (RSDs) between 5% and 9%. The achieved limits of detection for all analytes were below 0.05 µg kg⁻¹. The applicability of the method for the analysis of routine samples was studied by the analysis of a set of commercial bread and breakfast cereal samples. In all analysed samples, benzo[a]pyrene (BAP) was the most prevalent PAH with the content between 0.09 and 0.30 µg kg⁻¹. On average, samples showed low levels of the sum of the four EU marker PAHs (ΣPAH4) that ranged between 0.11 and 0.22 µg kg⁻¹ for bread samples and between 0.23 and 0.87 µg kg⁻¹ for breakfast cereal samples. The developed method was found suitable for the determination of PAHs in cereal-based foods like cornflakes and breads with total relative fat contents below 3.5%.

KEYWORDS:

• Four EU marker PAHs
• bread
• cornflakes
• GC/MS analysis
• method validation

Disclosure statement

No potential conflict of interest was reported by the authors.

Additional information

Funding

Sibel Kacmaz thanks TUBITAK (The Scientific and Technological Research Council of Turkey) BIDEB-2219 international postdoctoral research fellowship programme for financial support for the project, and the European Commission’s Joint Research Centre, Institute for Reference Materials and Measurements, for hosting the project.