Application of fully automated online solid phase extraction-liquid chromatography-electrospray-tandem mass spectrometry for the determination of sulfonamides and their acetylated metabolites in groundwater

The present study describes an automated methodology based on a liquid chromatography-electrospray, tandem mass spectrometry method combined with online solid phase extraction (online SPE-LC-ESI-MS/MS) for the simultaneous analysis of 16 sulfonamides (SAs) and five of their acetylated metabolites in groundwater. The evaluation of the degree of SA pollution in groundwater was made through the analysis of a total of 39 samples taken in seven groundwater bodies of Catalonia (Spain). Recovery values obtained ranged from 34.3% (N4-acetylsulfadiazine) to 134.4% (sulfabenzamide). The method limits of detection for all the analytes were 0.09–11 ng L−1. Sulfamethoxazole was the SA detected more frequently (56.4% of the samples), with an average concentration of 2.3 ng L−1, followed by sulfadimethoxine, present in 54% of the samples with an average concentration of 0.2 ng L−1. It should be highlighted that the acetylated metabolites were ubiquitous in the different samples, with frequencies of detection up to 36% and maximum concentrations of 18 ng L−1 (N4-acetylsulfamerazine).

[1]  A. G. Norman.  Advances in Agronomy , 1948, Nature.

[2]  E. Thurman,et al.  Analysis of trace levels of sulfonamide and tetracycline antimicrobials in groundwater and surface water using solid-phase extraction and liquid chromatography/mass spectrometry. , 2001, Analytical chemistry.

[3]  Sören Thiele-Bruhn,et al.  Pharmaceutical antibiotic compounds in soils – a review , 2003 .

[4]  Walter Giger,et al.  Trace determination of macrolide and sulfonamide antimicrobials, a human sulfonamide metabolite, and trimethoprim in wastewater using liquid chromatography coupled to electrospray tandem mass spectrometry. , 2004, Analytical chemistry.

[5]  Alistair B.A. Boxall,et al.  Veterinary medicines in the environment. , 2004 .

[6]  H. Singer,et al.  Fully automated online solid phase extraction coupled directly to liquid chromatography-tandem mass spectrometry. Quantification of sulfonamide antibiotics, neutral and acidic pesticides at low concentrations in surface waters. , 2005, Journal of chromatography. A.

[7]  H. Nau,et al.  Different behavior of tetracyclines and sulfonamides in sandy soils after repeated fertilization with liquid manure , 2005, Environmental toxicology and chemistry.

[8]  M. Kaštelan-macan,et al.  Solid phase extraction and HPLC determination of veterinary pharmaceuticals in wastewater. , 2006, Talanta.

[9]  M. A. Mohd,et al.  Determination of sulfonamides in selected Malaysian swine wastewater by high-performance liquid chromatography. , 2006, Journal of Chromatography A.

[10]  D. Aga,et al.  Occurrence of sulfonamide antimicrobials in private water wells in Washington County, Idaho, USA. , 2006, Chemosphere.

[11]  Adriano Joss,et al.  Fate of sulfonamides, macrolides, and trimethoprim in different wastewater treatment technologies. , 2007, The Science of the total environment.

[12]  D. Barceló,et al.  Wastewater treatment plants as a pathway for aquatic contamination by pharmaceuticals in the Ebro river basin (Northeast Spain) , 2007, Environmental toxicology and chemistry.

[13]  Maria S. Sepúlveda,et al.  Agricultural Contributions of Antimicrobials and Hormones on Soil and Water Quality , 2007 .

[14]  Damià Barceló,et al.  Highly sensitive simultaneous determination of sulfonamide antibiotics and one metabolite in environmental waters by liquid chromatography-quadrupole linear ion trap-mass spectrometry. , 2008, Journal of chromatography. A.

[15]  A. Schäffer,et al.  Fate in soil of 14C-sulfadiazine residues contained in the manure of young pigs treated with a veterinary antibiotic , 2008, Journal of environmental science and health. Part. B, Pesticides, food contaminants, and agricultural wastes.

[16]  Sören Thiele-Bruhn,et al.  Alterations in soil microbial activity and N-transformation processes due to sulfadiazine loads in pig-manure. , 2008, Environmental pollution.

[17]  Satish C. Gupta,et al.  Antibiotic losses in leaching and surface runoff from manure-amended agricultural land. , 2008, Journal of environmental quality.

[18]  Yan-xin Wang,et al.  Analysis of veterinary antibiotic residues in swine wastewater and environmental water samples using optimized SPE-LC/MS/MS. , 2009, Chemosphere.

[19]  M. Laušević,et al.  Determination of multiple pharmaceutical classes in surface and ground waters by liquid chromatography-ion trap-tandem mass spectrometry. , 2009, Journal of chromatography. A.

[20]  Roy Kasteel,et al.  Transport of Manure‐Based Applied Sulfadiazine and Its Main Transformation Products in Soil Columns , 2009 .

[21]  M. Matthies,et al.  A conceptual model describing the fate of sulfadiazine and its metabolites observed in manure-amended soils. , 2009, Chemosphere.

[22]  D. Ronen,et al.  Sulfamethoxazole contamination of a deep phreatic aquifer. , 2009, The Science of the total environment.

[23]  D. Barceló,et al.  Determination of 19 sulfonamides in environmental water samples by automated on-line solid-phase extraction-liquid chromatography-tandem mass spectrometry (SPE-LC-MS/MS). , 2010, Talanta.

[24]  D. Barceló,et al.  Simultaneous occurrence of nitrates and sulfonamide antibiotics in two ground water bodies of Catalonia (Spain) , 2010 .

[25]  T. DeSutter,et al.  Development of an ultra-high-pressure liquid chromatography-tandem mass spectrometry multi-residue sulfonamide method and its application to water, manure slurry, and soils from swine rearing facilities. , 2010, Journal of chromatography. A.