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Simultaneous extraction and determination of fluoroquinolones, tetracyclines and sulfonamides antibiotics in soils using optimised solid phase extraction chromatography-tandem mass spectrometry

An analytical method was developed for the simultaneous extraction and determination of 18 fluoroquinolones (FQs), tetracyclines (TCs) and sulfonamides (SAs) antibiotics from soils using solid phase extraction and liquid chromatography-tandem mass spectrometry. The soils were extracted by different solvents with the help of mechanical shaking and ultrasonic treatment at 59 kHz, followed by a strong anion exchange (SAX) cartridge to clean up soil samples and a hydrophilic lipophilic balance (HLB) cartridge as enrichment. The method was evaluated by testing the following variables: extraction solvents, the type of SPE cartridges, solvent volumes, initial spiking levels and soil types (silty clay loam and clay loam soils). The soil extraction method was validated using these two types of soils, representing two typical agricultural soils in northern China. For 2 g soil, the extraction steps with the mixture of potassium phosphate buffer and acetonitrile (ACN) (1/1, v/v, pH 3.2) provided satisfactory recoveries. In the clay loam soil, the recoveries of all the compounds were from 56% to 89% at the spiking level of 50 µg kg−1 soil, and from 69% to 97% at the spiking level of 200 µg kg−1 soil, respectively. Recoveries in silty clay loam soil were similar to that in clay loam. The method was successfully employed using soil samples collected from a farmland and afforestion area irrigated with sewage in northern China. The result indicates that trace antibiotics in sewage may accumulate in soil irrigated by river water containing sewage.