PMID- 16822516 OWN - NLM STAT- MEDLINE DCOM- 20090417 LR - 20191210 IS - 1873-3778 (Electronic) IS - 0021-9673 (Linking) VI - 1130 IP - 1 DP - 2006 Oct 13 TI - Determination of antimicrobials in sludge from infiltration basins at two artificial recharge plants by pressurized liquid extraction-liquid chromatography-tandem mass spectrometry. PG - 72-82 AB - 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. FAU - Diaz-Cruz, M Silvia AU - Diaz-Cruz MS AD - Department of Environmental Chemistry, Instituto de Investigaciones Quimicas y Ambientales, Consejo Superior de Investigaciones Cientificas, c/Jordi Girona 18-26, 08034 Barcelona, Spain. sdcqam@cid.csic.es FAU - Lopez de Alda, Maria Jose AU - Lopez de Alda MJ FAU - Barcelo, Damia AU - Barcelo D LA - eng PT - Journal Article PT - Research Support, Non-U.S. Gov't PT - Validation Study DEP - 20060705 PL - Netherlands TA - J Chromatogr A JT - Journal of chromatography. A JID - 9318488 RN - 0 (Anti-Infective Agents) RN - 0 (Sewage) SB - IM MH - Anti-Infective Agents/*analysis MH - Chromatography, High Pressure Liquid/*methods MH - Denmark MH - Reproducibility of Results MH - Sensitivity and Specificity MH - Sewage/*analysis MH - Solid Phase Extraction/*methods MH - Spectrometry, Mass, Electrospray Ionization/methods MH - Sweden MH - Tandem Mass Spectrometry/*methods EDAT- 2006/07/11 09:00 MHDA- 2009/04/18 09:00 CRDT- 2006/07/11 09:00 PHST- 2006/03/14 00:00 [received] PHST- 2006/05/18 00:00 [revised] PHST- 2006/05/19 00:00 [accepted] PHST- 2006/07/11 09:00 [pubmed] PHST- 2009/04/18 09:00 [medline] PHST- 2006/07/11 09:00 [entrez] AID - S0021-9673(06)01075-2 [pii] AID - 10.1016/j.chroma.2006.05.076 [doi] PST - ppublish SO - J Chromatogr A. 2006 Oct 13;1130(1):72-82. doi: 10.1016/j.chroma.2006.05.076. Epub 2006 Jul 5.