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Determination of antimicrobials in sludge from infiltration basins at two artificial recharge plants by pressurized liquid extraction-liquid chromatography-tandem mass spectrometry.
J Chromatogr A. 2006 Oct 13; 1130(1):72-82.JC

Abstract

This work describes the optimization of a multi-residue analytical approach for the simultaneous determination of 11 antimicrobials (9 sulphonamides and 2 penicillins) in sludge from infiltration basins. The method is based on pressurized liquid extraction (PLE) followed by solid-phase extraction (SPE) for pre-concentration and purification, and analysis by liquid chromatography-tandem mass spectrometry using electrospray in the positive ionization mode (LC-(ESI+)-MS/MS). Limits of detections (LODs) between 1 pg/g and 0.2 ng/g and limits of quantifications (LOQs) between 5 pg/g and 0.6 ng/g were achieved. Good recovery values (57.6-104%) were obtained for sulfamethazine, sulfapyridine, sulfadiazine and sulfamethoxypyridazine, while medium recovery values (14-47%) were afforded for sulfadimethoxine, sulfathiazole and sulfamethoxazole. However, only a poor recovery (<1%) could be possible for both penicillins and two sulphonamides, namely nafcillin, dicloxacillin, sulfisoxazole and sulfamethizole. These low recoveries were attributed to the presence of ionic suppression effects (even after thorough extraction and purification) rather than to an inefficient extraction. The method developed was applied to the analysis of sludge samples from the infiltration basins of two artificial recharge plants located in Sweden and Denmark. All target compounds were found to be present in at least one sample. Sulfadimethoxine, nafcillin and dicloxacillin were detected in all the samples analysed.

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Authors+Show Affiliations

Díaz-Cruz MS
Department of Environmental Chemistry, Instituto de Investigaciones Químicas y Ambientales, Consejo Superior de Investigaciones Científicas, c/Jordi Girona 18-26, 08034 Barcelona, Spain. sdcqam@cid.csic.es
López de Alda MJ
No affiliation info available
Barceló D
No affiliation info available

MeSH

Anti-Infective AgentsChromatography, High Pressure LiquidDenmarkReproducibility of ResultsSensitivity and SpecificitySewageSolid Phase ExtractionSpectrometry, Mass, Electrospray IonizationSwedenTandem Mass Spectrometry

Pub Type(s)

Journal Article
Research Support, Non-U.S. Gov't
Validation Study

Language

eng

PubMed ID

16822516

Citation

Díaz-Cruz, M Silvia, et al. "Determination of Antimicrobials in Sludge From Infiltration Basins at Two Artificial Recharge Plants By Pressurized Liquid Extraction-liquid Chromatography-tandem Mass Spectrometry." Journal of Chromatography. A, vol. 1130, no. 1, 2006, pp. 72-82.
Díaz-Cruz MS, López de Alda MJ, Barceló D. Determination of antimicrobials in sludge from infiltration basins at two artificial recharge plants by pressurized liquid extraction-liquid chromatography-tandem mass spectrometry. J Chromatogr A. 2006;1130(1):72-82.
Díaz-Cruz, M. S., López de Alda, M. J., & Barceló, D. (2006). Determination of antimicrobials in sludge from infiltration basins at two artificial recharge plants by pressurized liquid extraction-liquid chromatography-tandem mass spectrometry. Journal of Chromatography. A, 1130(1), 72-82.
Díaz-Cruz MS, López de Alda MJ, Barceló D. Determination of Antimicrobials in Sludge From Infiltration Basins at Two Artificial Recharge Plants By Pressurized Liquid Extraction-liquid Chromatography-tandem Mass Spectrometry. J Chromatogr A. 2006 Oct 13;1130(1):72-82. PubMed PMID: 16822516.
* Article titles in AMA citation format should be in sentence-case
TY - JOUR T1 - Determination of antimicrobials in sludge from infiltration basins at two artificial recharge plants by pressurized liquid extraction-liquid chromatography-tandem mass spectrometry. AU - Díaz-Cruz,M Silvia, AU - López de Alda,María José, AU - Barceló,Damià, Y1 - 2006/07/05/ PY - 2006/03/14/received PY - 2006/05/18/revised PY - 2006/05/19/accepted PY - 2006/7/11/pubmed PY - 2009/4/18/medline PY - 2006/7/11/entrez SP - 72 EP - 82 JF - Journal of chromatography. A JO - J Chromatogr A VL - 1130 IS - 1 N2 - This work describes the optimization of a multi-residue analytical approach for the simultaneous determination of 11 antimicrobials (9 sulphonamides and 2 penicillins) in sludge from infiltration basins. The method is based on pressurized liquid extraction (PLE) followed by solid-phase extraction (SPE) for pre-concentration and purification, and analysis by liquid chromatography-tandem mass spectrometry using electrospray in the positive ionization mode (LC-(ESI+)-MS/MS). Limits of detections (LODs) between 1 pg/g and 0.2 ng/g and limits of quantifications (LOQs) between 5 pg/g and 0.6 ng/g were achieved. Good recovery values (57.6-104%) were obtained for sulfamethazine, sulfapyridine, sulfadiazine and sulfamethoxypyridazine, while medium recovery values (14-47%) were afforded for sulfadimethoxine, sulfathiazole and sulfamethoxazole. However, only a poor recovery (<1%) could be possible for both penicillins and two sulphonamides, namely nafcillin, dicloxacillin, sulfisoxazole and sulfamethizole. These low recoveries were attributed to the presence of ionic suppression effects (even after thorough extraction and purification) rather than to an inefficient extraction. The method developed was applied to the analysis of sludge samples from the infiltration basins of two artificial recharge plants located in Sweden and Denmark. All target compounds were found to be present in at least one sample. Sulfadimethoxine, nafcillin and dicloxacillin were detected in all the samples analysed. SN - 1873-3778 UR - https://www.unboundmedicine.com/medline/citation/16822516/Determination_of_antimicrobials_in_sludge_from_infiltration_basins_at_two_artificial_recharge_plants_by_pressurized_liquid_extraction_liquid_chromatography_tandem_mass_spectrometry_ L2 - https://linkinghub.elsevier.com/retrieve/pii/S0021-9673(06)01075-2 DB - PRIME DP - Unbound Medicine ER -
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