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

TY - JOUR

T1 - Determination of sulfadiazine in phosphate- and DOC-rich agricultural drainage water using solid-phase extraction followed by liquid chromatography-tandem mass spectrometry

AU - Bouyou, P.A. Léon

AU - Weisser, Johan Juhl

AU - Strobel, Bjarne W.

PY - 2014/8

Y1 - 2014/8

N2 - 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 r 2∈=∈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. [Figure not available: see fulltext.]

AB - 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 r 2∈=∈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. [Figure not available: see fulltext.]

KW - Soil chemistry

KW - sulfadiazine

KW - UPLC-ESI-MS/MS

KW - DRAINAGE SYSTEMS

KW - Water Pollutants, Chemical

KW - analytical chemistry

KW - ???Miljøvenlig afgrødeproduktion???

KW - Phosphate

KW - Environmental Chemistry

U2 - 10.1007/s00216-014-7921-6

DO - 10.1007/s00216-014-7921-6

M3 - Journal article

C2 - 24912991

SN - 1618-2642

VL - 406

SP - 5019

EP - 5030

JO - Analytical and Bioanalytical Chemistry

JF - Analytical and Bioanalytical Chemistry

ER -