DETERMINATION OF SULFADIAZINE AND TRIMETHOPRIM IN MARINE SEDIMENT BY LC-APCI-MS

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Abstract
A liquid chromatographic method based on mass spectrometric detection using atmospheric pressure chemical ionisation (LC-APCI-MS) was developed for simultaneous determination of sulfadiazine and trimethoprim in marine sediment. Sediment was extracted with acetonitrile and cleaned up by solid phase extraction (SPE) on cationic and polymeric sorbents. Ion monitoring was performed using the protonated molecular ions for sulfadiazine (m/z 251) and trimethoprim (m/z 291). The limit of detection was 4 μg/kg for sulfadiazine and 0.9 μg/kg for trimethoprim. The recoveries were 72 ± 3% (mean ± SD) for sulfadiazine at a level of 100 μg/kg and 83 ± 4% for trimethoprim at a level of 25 μg/kg. The relative repeatability standard deviation was less than 6% at levels of 50 μg/kg for sulfadiazine and 20 μg/kg for trimethoprim.