Full
Outline
To establish a method for determination of fipronil and its metabolites in meat by amino functionalized magnetic nanomaterials purification-high performance liquid chromatography-mass spectrometry.
The samples were ultrasonically extracted with acetonitrile-water. The extract was purified by amino-functionalized magnetic nanoparticles, and then concentrated under nitrogen. The residue was dissolved in acetonitrile-water (7:3, V:V) to a final volume. The analyte solution was analyzed using a C18 column with methanol and water as the mobile phase under negative electrospray ionization mode. The data was collected using the multi reaction monitoring mode. The samples were analyzed based on the external standard method.
Under the established conditions, the target substances were well separated and showed a good linear relationship within the range of 1.0–20.0 ng/mL, with a correlation coefficient (r2) greater than 0.99. The limit of detection was 0.2 µg/kg and the limit of quantitation was 0.5 µg/kg. Through spiked recovery experiments, the recovery rates at 3 spiked levels ranged from 79.94% to 94.52%, with relative standard deviations of 2.95% to 8.22%.
Compared with traditional pretreatment methods, the proposed method utilizes a magnetic suction frame to absorb magnetism,which can eliminate the centrifugation steps, save time, ensure good reproducibility and reduce detection costs. The proposed method can be used to determine fipronil and its metabolites in meat. The establishment method can provide technical support for monitoring the residues of fipronil and its metabolites in meat on the market supervision.
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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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