PMID- 17683740 OWN - NLM STAT- MEDLINE DCOM- 20070831 LR - 20131121 IS - 1873-4324 (Electronic) IS - 0003-2670 (Linking) VI - 597 IP - 2 DP - 2007 Aug 6 TI - Quantitative analysis of clavulanic acid in porcine tissues by liquid chromatography combined with electrospray ionization tandem mass spectrometry. PG - 282-9 AB - The purpose of this study was to develop and validate a method for the determination of clavulanic acid (CLAV) residues in edible tissues of swine by liquid chromatography-electrospray ionisation-tandem mass spectrometry (LC-ESI-MS/MS). After a simple extraction of CLAV using an aqueous phosphate buffer solution of pH 6.0, an ultrafiltration step was performed for protein removal. Chromatography of CLAV and the internal standard tazobactam (TAZO) was achieved on a reversed-phase PLRP-S polymeric column (150 mm x 2.1 mm i.d., 100 A) using a mixture of 0.05 (v/v)% formic acid in water and acetonitrile. The mass spectrometer was operated in the MS/MS selected reaction monitoring (SRM) mode. The method was validated for the analysis of porcine muscle, skin plus fat, liver and kidney, according to the requirements defined by the European Community. Calibration curves were prepared for all tissues and good linearity was achieved over the concentration ranges tested (correlation coefficient > or = 0.99 and goodness-of-fit coefficient < or = 10%). Limits of quantification of 50 ng g(-1) were obtained for the analysis of CLAV in the various tissues which corresponds in all cases to at least half the maximum residue limits (MRLs). Limits of detection ranged between 8.0 and 15.14 ng g(-1). The within-day, between-day precisions and trueness fell within the ranges specified in the EMEA/CVMP/573-00/FINAL document. Biological samples from pigs that received an oral or intravenous bolus of a commercial amoxicillin/clavulanic acid formulation were analyzed using the described method. FAU - Reyns, Tim AU - Reyns T AD - Ghent University, Faculty of Veterinary Medicine, Department of Pharmacology, Toxicology, Biochemistry and Organ Physiology, Salisburylaan 133, B-9820 Merelbeke, Belgium. Tim.Reyns@UGent.be FAU - De Boever, Sandra AU - De Boever S FAU - De Baere, Siegrid AU - De Baere S FAU - De Backer, Patrick AU - De Backer P FAU - Croubels, Siska AU - Croubels S LA - eng PT - Journal Article DEP - 20070705 PL - Netherlands TA - Anal Chim Acta JT - Analytica chimica acta JID - 0370534 RN - 23521W1S24 (Clavulanic Acid) SB - IM MH - Animals MH - Chromatography, Liquid/*methods MH - Clavulanic Acid/*analysis/chemistry MH - Molecular Structure MH - Organ Specificity MH - Sensitivity and Specificity MH - Spectrometry, Mass, Electrospray Ionization/*methods MH - Swine MH - Tandem Mass Spectrometry/*methods EDAT- 2007/08/09 09:00 MHDA- 2007/09/01 09:00 CRDT- 2007/08/09 09:00 PHST- 2007/05/21 00:00 [received] PHST- 2007/06/29 00:00 [revised] PHST- 2007/06/30 00:00 [accepted] PHST- 2007/08/09 09:00 [pubmed] PHST- 2007/09/01 09:00 [medline] PHST- 2007/08/09 09:00 [entrez] AID - S0003-2670(07)01155-5 [pii] AID - 10.1016/j.aca.2007.06.056 [doi] PST - ppublish SO - Anal Chim Acta. 2007 Aug 6;597(2):282-9. doi: 10.1016/j.aca.2007.06.056. Epub 2007 Jul 5.