Determination of volatile N-nitrosamines in meat products by microwave-assisted extraction coupled with dispersive micro solid-phase extraction and gas chromatography – Chemical ionisation mass spectrometry

A sensitive procedure, microwave-assisted extraction (MAE) coupled dispersive micro solid-phase extraction (D-μ-SPE), was developed to extract N-nitrosodimethylamine (NDMA) and other six volatile N-nitrosamines (NAms) from meat products. Parameters affecting the efficiency of MAE and D-μ-SPE were systematically investigated. For MAE, 5-g of a homogenised meat sample was extracted with 30 mL of a sodium hydroxide (0.025 M) solution at 100 °C for 10 min. The optimum D-μ-SPE conditions were immersing 100 mg of Carboxen™ 1000 adsorbent in the MAE extract. After vigorously shaking for 30 min, the NAms were then desorbed by treatment with 200 μL of dichloromethane. A 10 μL aliquot was determined by gas chromatography with chemical ionisation mass spectrometry (GC–CI-MS) using the selected-ion-storage (SIS) mode. The limits of quantitation (LOQs) were 0.03–0.36 ng/g. Preliminary results revealed that NDMA was present in the highest concentration, ranging from 0.8 to 3.2 ng/g.