Objective To establish an analytical method for the simultaneous determination of 6 kinds of fluoroquinolones and 4 kinds of benzodiazepines residues in aquatic products by ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). Methods Aquatic product samples were extracted with 1% formic acid in acetonitrile. The extracts were concentrated with a rotary evaporator and then reconstituted in 90% acetonitrile aqueous solution (containing 1% formic acid), and purified through a pass-through solid phase extraction cartridge (ProElut PLS-A). The purified extracts were directly analyzed by UPLC-MS/MS. Quantification was performed using the isotope internal standard method. Results The 10 kinds of target compounds exhibited good linearity within the concentration range of 0.5 to 50.0 ng/mL, with correlation coefficients (r) all greater than 0.998. The limits of quantitation for these compounds in 5 kinds of different aquatic product matrices ranged from 0.5 to 1.0 μg/kg. The recovery rates at low, medium and high spiking levels ranged from 81.5% to 109.7%, with relative standard deviations ranging from 0.24% to 13.22%. Conclusion Methodological validation confirmed that the developed method is highly sensitive, accurate in quantification, stable, and straightforward in operation. It is suitable for high-throughput detection of 6 kinds of fluoroquinolones and 4 kinds of benzodiazepines residues in aquatic products.
| 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 |