To develop a method for the simultaneous determination of 30 kinds of pesticide and veterinary drug residues across 10 classes-including sulfonamides, tetracyclines, quinolones, macrolides, nitroimidazoles, triphenylmethanes, β-lactams, hormones, organophosphorus compounds and carbamates in aquatic products by automated solid-phase extraction coupled with ultra performance liquid chromatography-tandem mass spectrometry.
Samples were extracted with acetonitrile containing formic acid, purified using HLB solid-phase extraction cartridges, and separated on a Waters ACQUITY UPLC BEH C18 column with a mobile phase consisting of 0.1% formic acid in acetonitrile and 0.1% formic acid in water, and analyzed by a SCIEX\Triple Quad 5500+ tandem mass spectrometer.
The 30 kinds of compounds exhibited good linearity within the concentration range of 5–100 μg/L, with correlation coefficients ranging from 0.9914 to 0.9998. The limits of detection were less than or equal to 0.025 mg/kg, and the limits of quantitation were less than or equal to 0.050 mg/kg. Mean recoveries for spiked samples ranged from 62.8% to 108.1%, with relative standard deviations of 1.0%–14.7% (n=6).
The method demonstrates high precision, good accuracy and a high degree of automation, making it suitable for high-throughput screening of pesticide and veterinary drug residues in aquatic products.
| 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 |