To establish a method for the simultaneous determination of dexamethasone, betamethasone, florfenicol and florfenicol amine residues in pork and beef by high performance liquid chromatography-tandem mass spectrometry.
The samples were extracted with acetonitrile and purified using the QuEChERS method. Separation was performed on a BEH-C18 column with acetonitrile and ultrapure water as the mobile phase for gradient elution. Qualitative and quantitative analysis was conducted via multiple reaction monitoring under both positive and negative ion scanning modes using the external standard method.
Dexamethasone, betamethasone, florfenicol and florfenicol amine exhibited excellent linearity within the mass concentration range of 0.2–100.0 ng/mL, with correlation coefficients exceeding 0.9990. The recovery rates ranged from 85.1% to 107.5%. The limits of detection (LODs) for dexamethasone were 0.44–0.48 μg/kg and the limits of quantitation (LOQs) were 1.45–1.58 μg/kg. For betamethasone, the LODs were 0.46–0.51 μg/kg and the LOQs were 1.52–1.68 μg/kg. For florfenicol, the LODs were 0.47–0.58 μg/kg and LOQs were 1.55–1.91 μg/kg. For florfenicol amine, the LODs were 0.40–0.45 μg/kg and the LOQs were 1.32–1.49 μg/kg.
This method demonstrates accurate parameter determination, with excellent recovery rates, high precision, and a simple, convenient pretreatment process. It meets the requirements for simultaneous screening and qualitative and quantitative detection of dexamethasone, betamethasone, florfenicol and florfenicol amine residues in pork and beef, thereby providing a reliable tool for routine risk assessment.
| 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 |