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Objective To develope a method based on organic solvent extraction and solid phase extraction purification combined with ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) for the simultaneous determination of 23 kinds of perfluorinated and polyfluoroalkyl substances (PFASs), including perfuluorocarboxylic acids, perfluoroalkyl sulfonic acids, and fluorotelomer sulfonic acids, in freshwater fishes. Methods The chromatographic conditions and mass spectrometry parameters were optimized, and the effects of extraction solvent and solid phase extraction column fillers on sample recovery and purification were investigated. The optimal sample pretreatment and instrument conditions were determined. Freshwater fish samples were directly extracted with 2% formic acid and purified using a lipid removal PPR Pro column. With 5 mmol/L ammonium formate aqueous solution and methanol as mobile phase, the target substances were separated by C18 chromatographic column. The mass spectrum was detected by electrospray ion source (ESI-), multi reaction monitoring (MRM) and stable isotope internal standard method. Results The 23 kinds of target PFASs had a good linear relationship within 0.5-100.0 ng/mL mass concentration range (r2>0.980), with the limits of detection was 0.030-0.146 μg/kg and the limits of quantification were 0.100-0.567 μg/kg. The spiked recoveries of serum sample were 72.9%-111.0%, with relative standard deviations of 3.0%-17.5% (n=9). Conclusion The method has the advantages of simple operation, high sensitivity, strong anti-interference and good precision, and is suitable for the rapid detection and analysis of 23 kinds of perfluoroalkyl carboxylic acids, perfluoroalkyl sulfonic acid and polyfluorotelomeric sulfonic acid in freshwater fish.
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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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