PMID- 18804772 OWN - NLM STAT- MEDLINE DCOM- 20090112 LR - 20090115 IS - 0021-9673 (Print) IS - 0021-9673 (Linking) VI - 1209 IP - 1-2 DP - 2008 Oct 31 TI - Multi-class determination of antimicrobials in meat by pressurized liquid extraction and liquid chromatography-tandem mass spectrometry. PG - 162-73 LID - 10.1016/j.chroma.2008.09.011 [doi] AB - A multi-residue method using pressurized liquid extraction (PLE) and liquid chromatography-tandem mass spectrometry (LC-MS/MS) has been developed for determining trace levels of 31 antimicrobials, including beta-lactams, lincosamides, macrolides, quinolones, sulfonamides, tetracyclines, nitroimidazoles and trimethoprim. The extraction method required pre-homogeneization of the meat with EDTA-washed sand and subsequent one-static-cycle extraction for 10 min with 40 ml of water at 1500 psi and 70 degrees C. The effect of operation temperature, pressure, flush volume, and static cycles on PLE performance was studied. Average recoveries ranged from 75 to 99% with relative standard deviations <18%. The method was validated according to the European Union requirements (2002/657/EC). In addition to the quality parameters included in that decision, the limits of detection (LODs) and quantification (LOQs) were determined. The use of LC-MS/MS provided LODs (between 3 and 15 microg kg(-1)) and LOQs (between 10 and 50 microg kg(-1)), by far lower than half of their maximum residue limits (MRLs) (between 50 and 1200 microg kg(-1)). Confirmation of the presence of any of the studied compounds was accomplished in 1h after sample receipt. This methodology has been successfully applied to the analysis of cattle and pig tissue samples from local markets and slaughterhouses of the Valencian Community (Spain). The results showed the presence of some antimicrobials at different concentrations. Quinolones and tetracyclines were the antimicrobials most detected in cattle and pig samples, respectively. Sulfonamides were also frequently detected in both types of samples. FAU - Carretero, Vanesa AU - Carretero V AD - Laboratori de Bromatologia i Toxicologia, Facultat de Farmacia, Universitat de Valencia, Av. Vicent Andres Estelles s/n, 46100 Burjassot, Valencia, Spain. FAU - Blasco, Cristina AU - Blasco C FAU - Pico, Yolanda AU - Pico Y LA - eng PT - Journal Article PT - Research Support, Non-U.S. Gov't DEP - 20080907 PL - Netherlands TA - J Chromatogr A JT - Journal of chromatography. A JID - 9318488 RN - 0 (Anti-Bacterial Agents) SB - IM MH - Animals MH - Anti-Bacterial Agents/*analysis/chemistry/isolation & purification MH - Cattle MH - Chromatography, Liquid/*methods MH - Meat/*analysis MH - Molecular Structure MH - Reproducibility of Results MH - Swine MH - Tandem Mass Spectrometry/*methods EDAT- 2008/09/23 09:00 MHDA- 2009/01/13 09:00 CRDT- 2008/09/23 09:00 PHST- 2008/06/23 00:00 [received] PHST- 2008/08/31 00:00 [revised] PHST- 2008/09/04 00:00 [accepted] PHST- 2008/09/23 09:00 [pubmed] PHST- 2009/01/13 09:00 [medline] PHST- 2008/09/23 09:00 [entrez] AID - S0021-9673(08)01525-2 [pii] AID - 10.1016/j.chroma.2008.09.011 [doi] PST - ppublish SO - J Chromatogr A. 2008 Oct 31;1209(1-2):162-73. doi: 10.1016/j.chroma.2008.09.011. Epub 2008 Sep 7.