To develop a method for determination of fluindapyr, flutianil and fenpicoxamid in the milk and formula by liquid chromatography-tandem mass spectrometry.
The samples were extracted by ultrasonic vortexing with acetonitrile. The analysis solution was purified by QuEChERS dSPE EMR-Lipid lipid removal tubes, and then centrifuged and filtered before being analyzed. The test method used acetonitrile and 0.1% formic acid water as the mobile phase, with a flow rate of 0.3 mL/min. A gradient elution program was applied, and the separation was carried out on a Shim-pack GIST-HP C18-AQ chromatographic column. The detection was performed in positive ion mode with electrospray ionization and multiple reaction monitoring mode. Quantification was conducted using the matrix-matched external standard method.
For milk and milk powder matrices, there was a good linear relationship between the mass concentrations of fluindapyr, flutianil and fenpicoxamid ranging from 0.5 to 20.0 ng/mL and their corresponding peak areas, with R2 values all greater than or equal to 0.9993. At 3 kinds of different spiked levels of 0.005, 0.010 and 0.050 mg/kg, the average recoveries of fluindapyr, flutianil and fenpicoxamid were 86.3% to 105.9%, and the relative standard deviations were 3.96% to 9.18%.
This method can meet the requirements of accuracy, precision and sensitivity for the detection of fluindapyr, flutianil and fenpicoxamid in milk and milk powder.
| 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 |