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Objective To establish an analytical method for the determination of gamithromycin residues in raw milk based on matrix external standard method combined with through type purification column (EMR-Lipid) and high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS). Methods The samples were extracted with acid acetonitrile, purified by the EMR-Lipid through type purification column, gradient eluted through a BEH C18 chromatographic column. Detection was carried out in the electrospray positive ion multiple reaction mode, and quantification was performed using the matrix external standard method. Results Calibration curves were linear in the range of 0.5-20.0 ng/mL with correlation coefficients more than 0.99. The limit of detection (LOD) was 0.5 μg/kg, limit of quantification (LOQ) was 1.0 μg/kg. Gamithromycin showed a matrix enhancement effects in raw milk. After matrix blank curve correction, the average recoveries of gamithromycin at different spiked concentrations ranged from 74.0% to 77.0%, and the relative standard deviations (RSD) of the determination results were from 3.92% to 4.57%. Conclusion This method is accurate, sensitive, stable, simple, and easy to operate, it can be used for the rapid determination and quantitative analysis of gamithromycin residues in raw milk, providing technical support for monitoring the residual amount of gamithromycin 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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