Determination of Eleven N-Nitrosamines in Animal Derived Foods by Gas Chromatography-Tandem Mass Spectrometry after Pass-Through Solid Phase Extraction

A method was developed for the determination of 11 N-nitrosamines in animal derived foods by pass-through solid phase extraction coupled to gas chromatography-tandem mass spectrometry (GC-MS/MS). The rehydrated samples were extracted with acetonitrile and rapidly purified by using a Prime HLB solid phase extraction column (200 mg/6 mL). The target compounds were detected in the multiple reaction monitoring (MRM) mode, and quantified by the matrix matched external standard method. The calibration curves for the 11 N-nitrosamines were linear in the concentration range of 0.5–500.0 ng/mL, with correlation coefficients of 0.9994–0.9998. The limits of detection (LODs) and the limits of quantitation (LOQs) were 0.2–0.3 and 0.5–1.0 μg/kg, respectively. The average recoveries at spiked levels of 1, 4 and 10 μg/kg ranged from 80.1% to 97.4%, and the relative standard deviations (RSDs) were between 2.3% and 8.8%. The extraction and purification time required by this method was only 15 min/sample and greatly shortened compared with GB 5009.26-2016, and the detection efficiency was increased by 10 times. This method allows rapid detection of N-nitrosamines residues in animal derived foods.