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Objective: To establish a method for the determination of veterinary drug residues in Galli Gigerii Endothelium Corneum by ultra high performance liquid chromatography-tandem triple quadrupole mass spectrometry (UPLC-QQQ MS/MS) with solid-phase extraction. Methods: The samples were evenly dispersed,extracted with acetonitrile and acetonitrile containing 0.5% formic acid, and cleaned up with Oasis PRiME HLB solid phase extraction columns. The extracts were separated on Agilent ZORBAX Eclipse Plus C18 (3.0 mm×150 mm, 1.8 μm) using 5 mmol · L-1 ammonium acetate and acetonitrile (containing 0.1% formic acid) as mobile phase by gradient elution. The detection of veterinary drug residues was detected by tandem mass spectrometry with positive electrospray ion source under multiple reaction monitoring (MRM) mode. The matrix-matched external standard method was used for the quantitation. Results: The method exhibited good linearities within a certain concentration range r≥0.995 8. The limits of detection (LODs) were in the range of 0.1-3 μg · kg-1. The limits of quantitation (LOQs) were in the range of 0.2-10 μg · kg-1. The good recovery values (61.9%-121.5%) were achieved for all the 68 veterinary drugs with RSDs ranging from 0.50% to 8.4% for spiking 3 different levels. Out of 50 batches of samples, 5 batches of Galli Gigerii Endothelium Corneum were found to contain veterinary drug residues,including amantadine, doxycycline, enrofloxacin, and florfenicol. Conclusion: This method proves suitable for the rapid determination of multiple veterinary drug residues in Galli Gigerii Endothelium Corneum, with a simple,quick, accurate and procedure.
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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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