To establish an analytical method for detection of residual tildipirosin in raw milk by high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS).
The sample was extracted with acid acetonitrile, purified by enhanced matrix removal (EMR) purification column, and then separated by BEH C18. The target compound was analyzed by a positive electrospray ion multiple reaction monitoring mode and quantitative analysis using matrix matching isotope internal standard method for quantification.
The calibration curves were linear in the range of 2.5–100.0 ng/mL with correlation coefficients more than 0.99. The limit of detection was 2.5 μg/kg, limit of quantitation was 5.0 μg/kg. The average recoveries at different addition concentrations ranged from 78.2% to 97.6%, with the relative stand deviations of the determination results ranged from 6.02% to 7.69%.
This method is accuracy, sensitive stability, simple and easy to operate, which can be used to determinate of residual amounts of tildipirosin in raw milk.
| 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 |