PMID- 23790854 OWN - NLM STAT- MEDLINE DCOM- 20140103 LR - 20191210 IS - 1873-7072 (Electronic) IS - 0308-8146 (Linking) VI - 141 IP - 2 DP - 2013 Nov 15 TI - An HPLC-DAD method for the simultaneous determination of nine beta-lactam antibiotics in ewe milk. PG - 829-34 LID - S0308-8146(13)00387-7 [pii] LID - 10.1016/j.foodchem.2013.02.131 [doi] AB - The presence of beta-lactam residues in foodstuffs constitutes a potential risk to the human health and undesirable effects on consumers, and nowadays these antibiotic residues are also recognised as an emerging environmental problem. In addition, these are of great concern to prestigious Manchego cheese processors (Central Spain denomination of origin) because they reduce the curdling of milk and cause improper cheese ripening, which consequently lead to an important loss of monetary income. This work describes the development of a sensitive and reliable method using liquid chromatography with UV-diode array detection (LC-DAD) for simultaneous determination of the beta-lactam antibiotics, ampicillin (AMP), benzylpenicillin (PEG), cephalexin (CFX), cefazolin (CFL), cefoperazone (CFP), cloxacillin (CLO), dicloxacillin (DCL), oxacillin (OXA) and phenoxymethylpenicillin (PEV), in Manchega ewe milk. The column, mobile phase, temperature and flow rate were optimised to provide the best resolution of these analytes. The extraction method of the antibiotic residues involves the deproteinisation of the milk sample using acetonitrile and centrifugation followed by a solid-phase extraction (SPE) clean-up. The recoveries for the studied beta-lactams ranged from 79% to 96% with relative standard deviations between 0.5% and 4.9%. The limits of quantification (LOQs) for all these compounds were in the range of 3.4-8.6mugkg(-1), which are lower than the maximum residue limits (MRLs) established by the European Union for the studied beta-lactams in milk, making the method suitable for performing routine analyses. The proposed multi-residue LC-UV-diode array detection (LC-DAD) method is a powerful and popular alternative for the determination and confirmation of antibiotic residues in small milk industries and is the first one capable of determining nine beta-lactam antibiotics in samples of Manchega ewe milk. CI - Copyright (c) 2013 Elsevier Ltd. All rights reserved. FAU - Camara, M AU - Camara M AD - Regional Centre of Animal Selection and Reproduction (CERSYRA), E-13300 Valdepenas, Spain. FAU - Gallego-Pico, A AU - Gallego-Pico A FAU - Garcinuno, R M AU - Garcinuno RM FAU - Fernandez-Hernando, P AU - Fernandez-Hernando P FAU - Durand-Alegria, J S AU - Durand-Alegria JS FAU - Sanchez, P J AU - Sanchez PJ LA - eng PT - Evaluation Study PT - Journal Article PT - Research Support, Non-U.S. Gov't DEP - 20130328 PL - England TA - Food Chem JT - Food chemistry JID - 7702639 RN - 0 (Anti-Bacterial Agents) RN - 0 (beta-Lactams) SB - IM MH - Animals MH - Anti-Bacterial Agents/*analysis MH - Chromatography, High Pressure Liquid/instrumentation/*methods MH - Food Contamination/*analysis MH - Milk/*chemistry MH - beta-Lactams/*analysis EDAT- 2013/06/26 06:00 MHDA- 2014/01/05 06:00 CRDT- 2013/06/25 06:00 PHST- 2011/03/04 00:00 [received] PHST- 2012/10/24 00:00 [revised] PHST- 2013/02/22 00:00 [accepted] PHST- 2013/06/25 06:00 [entrez] PHST- 2013/06/26 06:00 [pubmed] PHST- 2014/01/05 06:00 [medline] AID - S0308-8146(13)00387-7 [pii] AID - 10.1016/j.foodchem.2013.02.131 [doi] PST - ppublish SO - Food Chem. 2013 Nov 15;141(2):829-34. doi: 10.1016/j.foodchem.2013.02.131. Epub 2013 Mar 28.