Analytical and Bioanalytical Chemistry

, Volume 406, Issue 20, pp 5019–5030 | Cite as

Determination of sulfadiazine in phosphate- and DOC-rich agricultural drainage water using solid-phase extraction followed by liquid chromatography-tandem mass spectrometry

  • P. A. Léon Bouyou
  • Johan J. Weisser
  • Bjarne W. Strobel
Research Paper


Trace levels of the veterinary antibiotic compound sulfadiazine (SDZ) can be determined in agricultural drainage water samples with this new method. Optimized sample pretreatment and solid-phase extraction was combined with liquid chromatography coupled to tandem mass spectrometry (SPE LC-MS/MS) using positive electrospray ionization. The linear dynamic range for the LC-MS/MS was assessed from 5 μg/L to 25 mg/L with a 15-point calibration curve displaying a coefficient of correlation r2 = 0.9915. Agricultural drainage water spiked at a concentration of 25 ng/L gave recoveries between 63 and 98 % (relative standard deviation 15 %), while at 10 ng/L, it showed a lower recovery of 32 % (relative standard deviation 47 %). The final SPE LC-MS/MS method had a limit of detection (LOD)Method and a limit of quantification (LOQ)Method of 7.5 and 23 ng/L agricultural drainage water, respectively. Determination of SDZ, spiked at a realistic concentration of 50 μg/L, in artificial drainage water (ADW) containing common and high levels of phosphate (0.05, 0.5, and 5 mg/L) gave recoveries between 70 and 92 % (relative standard deviation 7.4–12.9 %). Analysis of the same realistic concentration of SDZ in ADW, spiked with common and high levels of dissolved organic carbon (2, 6, and 15 mg/L) confirmed the possible adaptation of a tandem solid-phase extraction (strong anion exchange (SAX)-hydrophilic-lipophilic balance (HLB)) followed by liquid chromatography-tandem mass spectrometry methodology. Recoveries obtained ranged from 104 to 109 % (relative standard deviation 2.8–5.2 %). The new methods enable determination of the veterinary antibiotic compound SDZ in agricultural drainage water from field experiments and monitoring schemes for phosphate- and dissolved organic carbon (DOC)-rich water samples in intensive farming areas.


Clean-up and up-concentration of sulfadiazine from agricultural drainage water


SDZ LC-MS/MS SPE Veterinary antibiotic Sulfonamide 


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Copyright information

© Springer-Verlag Berlin Heidelberg 2014

Authors and Affiliations

  • P. A. Léon Bouyou
    • 1
  • Johan J. Weisser
    • 2
  • Bjarne W. Strobel
    • 1
  1. 1.Section of Environmental Chemistry and Physics, Department of Plant and Environmental SciencesUniversity of CopenhagenFrederiksbergDenmark
  2. 2.Section of Analytical Biosciences, Department of PharmacyUniversity of CopenhagenCopenhagenDenmark

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