Microwave assisted saponification (MAS) followed by on-line liquid chromatography (LC)–gas chromatography (GC) for high-throughput and high-sensitivity determination of mineral oil in different cereal-based foodstuffs

• MOSH and MOAH determination in cereal-based products.
• Microwave assisted saponification and extraction followed by on-line LC–GC.
• Method performance and recovery tests on different matrices.
• Comparison with other extraction methods.
• Applications to dry pasta, bread, biscuits and cakes.

A high throughput, high-sensitivity procedure, involving simultaneous microwave-assisted extraction (MAS) and unsaponifiable extraction, followed by on-line liquid chromatography (LC)–gas chromatography (GC), has been optimised for rapid and efficient extraction and analytical determination of mineral oil saturated hydrocarbons (MOSH) and mineral oil aromatic hydrocarbons (MOAH) in cereal-based products of different composition. MAS has the advantage of eliminating fat before LC–GC analysis, allowing an increase in the amount of sample extract injected, and hence in sensitivity. The proposed method gave practically quantitative recoveries and good repeatability. Among the different cereal-based products analysed (dry semolina and egg pasta, bread, biscuits, and cakes), egg pasta packed in direct contact with recycled paperboard had on average the highest total MOSH level (15.9 mg kg−1), followed by cakes (10.4 mg kg−1) and bread (7.5 mg kg−1). About 50% of the pasta and bread samples and 20% of the biscuits and cake samples had detectable MOAH amounts. The highest concentrations were found in an egg pasta in direct contact with recycled paperboard (3.6 mg kg−1) and in a milk bread (3.6 mg kg−1).