To establish an analytical method for the simultaneous determination of 36 kinds of veterinary drug residues (including 19 kinds of sulfonamides, 13 kinds of quinolones and 4 kinds of tetracyclines) in sea duck eggs by ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS).
Sea duck egg samples were extracted with 0.2 mL of 10% potassium ferrocyanide solution and 0.2 mL of 20% zinc acetate solution, and purified using an Oasis HLB solid-phase extraction column. Separation of the target analytes was performed on a Waters ACQUITY UPLC BEH C18 column using a gradient elution program. The mobile phase consisted of 0.1% formic acid aqueous solution and acetonitrile containing 0.1% formic acid data acquisition for qualitative and quantitative analysis was carried out in the positive electrospray ionization mode using multiple reaction monitoring, with quantification by the external standard method.
The linear correlations of sulfonamides, quinolones and tetracyclines were favorable in the concentration range of 5–250 μg/kg(r2≥0.9969). The average recoveries ranged from 87.8% to 101.2%, with relative standard deviations of 1.25%–4.53%. The limits of detection and limits of quantitation were 0.05–5.11 μg/kg and 0.18–17.04 μg/kg,respectively.
The established method is rapid, simple, sensitive and reliable, and is suitable for the simultaneous qualitative and quantitative detection of sulfonamide, quinolone and tetracycline veterinary drug residues in large batches of sea duck eggs.
| 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 |