Determination of Nine N-nitrosamines in Dried Aquatic Products by QuEChERS Gas Chromatography-triple Quadrupole Tandem Mass Spectrometry
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Abstract:
A method for the simultaneous determination of nine N-nitrosamines in dried aquatic products by gas chromatography-tandem mass spectrometry (GC-MS/MS) was established. After quick, easy, cheap, effective, rugged, and safe (QuEChERS) pretreatment, the samples were subjected to acetonitrile extraction, followed by the application of Agilent bond elut enhanced matrix removal-lipid (EMR-Lipid). The compounds of interest were separated by a HP-INNOWAX column (30 m×0.25 mm×0.25 μm). They were subsequently analyzed by GC-MS/MS in the multiple reaction monitoring mode (MRM) and quantified by an external standard method. The experimental results show good linearity for the nine N-nitrosamines in the range from 0.30 to 50.00 μg/L, with linear regression coefficients R2 higher than 0.999. The limits of detection are 0.3 μg/kg, and the limits of quantification are 1.0 μg/kg. The average recovery rates of the nine N-nitrosamines were between 80.41% and 113.73% when 1.00 μg/kg, 4.00 μg/kg, and 10.00 μg/kg of N-nitrosamines were added to dried squids, shrimps, oysters, and scallops. Meanwhile, the relative standard deviations (RSDs) were 1.34% to 11.80% (n=6). Different levels of N-nitrosodimethylamine, N-nitrosodiethylamine, N-nitrosodibutylamine, N-nitrosopyrrolidine, and N-nitrosodiphenylamine were detected in dried aquatic products available in the market. The proposed method enables simple pre-treatment, and it is inexpensive, highly sensitive, reasonably stable, and quantitatively accurate. It can rapidly determine and quantitatively analyze nine N-nitrosamines in dry aquatic products.
