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Objective To establish a new method for the determination of 4 kinds of non-volatile N-nitrosamines (NVNA), N-nitrosoproline (NPRO), N-nitrososarcosine (NSAR), N-nitroso-thiazolidine-4-carboxylic acid (NTCA) and N-nitroso-thiazolidine-4-carboxylic acid (NMTCA), in dried smoked fish products by liquid chromatography-tandem mass spectrometry. Methods The samples were extracted by acetonitrile, degreased with n-hexane, separated on a MORHCHEM Caprisil C18-AQ (4.6 mm×250 mm, 5 μm)column, and detected by liquid chromatography-tandem mass spectrometry (LC-MS/MS) in multiple reaction monitoring (MRM) mode, and quantified by the external standard method of matrix standard curve. Results The linearity of the 4 kinds of NVNA was good in ranges of 1,4,10 or 50-800 ng/mL with r2>0.996, the detection limits were 1.36-56.17 μg/kg, the quantification limits were 4.52-187.2 μg/kg, and the spiked recoveries of 4 kinds of NVNA ranged from 90.34%-103.60% with the relative standard deviations (RSDs) of 1.75%-6.47%. Practical applications showed that NVNAs were detected in commercially available samples of the dried smoked fish at different levels and in different species, with the weakly carcinogenic NSAR being detected at higher rates and levels. Conclusion This method is simple in sample pretreatment, good in accuracy and high in precision, which can meet the simultaneous determination of 4 kinds of NVNA in dried smoked fish, and provides a valuable technical reference for the regulation and control of the NVNA contamination level in dried smoked fish products.
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| 科 Family | 属数 Number of genus | 种数 Number of species | 占总种数比例 Percentage of total species (%) | 属 Genus | 种数 Number of species | 占总种数比例 Percentage of total species (%) |
|---|---|---|---|---|---|---|
| 鹅膏菌科Amanitaceae | 2 | 11 | 5.26 | 鹅膏菌属 Amanita | 10 | 4.78 |
| 小菇科 Mycenaceae | 2 | 12 | 5.74 | 丝盖伞属 Inocybe | 5 | 2.39 |
| 多孔菌科 Polyporaceae | 8 | 14 | 6.70 | 蜡蘑属 Laccaria | 5 | 2.39 |
| 红菇科 Russulaceae | 3 | 23 | 11.00 | 小皮伞属 Marasmius | 6 | 2.87 |
| 小菇属 Mycena | 11 | 5.26 | ||||
| 光柄菇属 Pluteus | 5 | 2.39 | ||||
| 红菇属 Russula | 17 | 8.13 | ||||
| 栓菌属 Trametes | 5 | 2.39 |
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