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Objective To establish a method for the simultaneous determination of fasciolicides and its metabolite (nitroxinil, rafoxanide, closantel, triclabendazole and ketotriclabendazole) in raw milk by QuEChERS coupled with ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). Methods The raw milk samples was extracted with 3% triethylamine acetonitrile-ethyl acetate acetate solution (7:3, V:V), purified by C18 adsorbent powder, and determined by UPLC-MS/MS with external standard method. The chromatographic separation was performed on an ZORBAX Eclipse Plus C18 (2.1 mm×100 mm 1.8 μm) column with a mobile phase of 0.1% formic acid-acetonitrile solution, and detected under multiple reaction monitoring (MRM) mode in the positive and negative electrospray ion modes. Results The results showed that a good linear relationship was obtained in the mass concentration range of 1 to 100 μg/L for fasciolicides and its metabolite, and the correlation coefficients (r) were all greater than 0.9988, the limits of detection were 2.5 μg/kg, and the limits of quantitation were 5 μg/kg. The average recoveries of 5 kinds of compounds at the concentration levels of 10, 20 and 100 μg/kg were between 86.0% and 108.2%, and the relative standard deviation ranged from 0.81% to 5.60%. Conclusion The method is simple, rapid accurate and reliable, and is suitable for the rapid determination of the residues of fasciolicides and its metabolite in raw milk.
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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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