Full
Outline
To establish a method for the determination of fenpicoxamid and florylpicoxamid residues (2 kinds of new types picolinamide pesticide) in vegetables and fruits by pipette-tip based modified QuEChERS-high performance liquid chromatography-tandem mass spectrometry.
The vegetable and fruit samples were extracted by shaking with acetonitrile assisted with QuEChERS salts, and purified using disposable tips packed with clean-up sorbents. The analytes were separated by a HPLC Shim-pack GIST C18 column (100 mm×2.1 mm, 2 μm) with acetonitrile-0.1% formic acid in water as the mobile phase by gradient elution mode. The target compounds were analyzed by high performance liquid chromatography-tandem mass spectrometry in multiple reaction monitoring mode, and quantified by the external standard method with matrix-matched calibration curves.
The linear relationship between the 2 kinds of pesticides was good within the mass concentration range of 1–40 ng/mL (correlation coefficient r>0.994), and the limits of quantitation were 0.01 mg/kg, could meet the requirements of residue detection. Method validation was conducted in 5 kinds of matrices including Wogan mandarin, celery, apple, scallion and raisin, and the average recovery rates at the spiked levels of 0.01–0.10 mg/kg were 62.6% to 119.1% with the relative standard deviation of 1.98% to 13.10%.
The proposed method is simple, rapid and efficient, and is suitable for the rapid screening and accurate quantitation of 2 kinds of novel picolinamide pesticide residues in vegetables and fruits.
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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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