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It is necessary to establish a sensitive, selective, efficient and accurate method for the simultaneous detection of multiple antibiotic residues in soil. In this study, the method of solid phase extraction-high performance liquid chromatography-tandem mass spectrometry (LC-MS/MS) for the determination of 20 antibiotics simultaneously in soil was established by optimizing the extraction conditions (extractant type, extraction method, shading and overnight) and the purification conditions (cartridge type). Under the optimized analysis conditions, the target antibiotics showed good linearity in the linear range of 0.10-100.00 μg/kg, with R2 ranging from 0.9951-0.9999. The recovery ratio ranged from 62%-116%, the relative standard deviation was 0.9%-16.8%, the limit of detection was 0.01-0.50 μg/kg, and the limit of quantification was 0.04-2.00 μg/kg. The method was applied for the detection of antibiotic residues in soil samples collected from greenhouse vegetable bases in Wuqing district, Tianjin, China. It showed that 4 classes of antibiotics were detected in the soil, and up to 16 of target antibiotics could be detected simultaneously. The total residual concentration of antibiotics in the soil varied from 2.52-142.00 μg/kg. The highest concentration of individual antibiotic was 105.00 μg/kg (oxytetracycline). The method established in the study is aim to provide reference for the formulation of the standard for the simultaneous detection of multiple antibiotic residues in soil and provide methodological basis for the prevention and control of emerging contaminants.
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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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