title: Determination of tetracyclines in pig and other meat samples using liquid chromatography coupled with diode array and tandem mass spectrometric detectors.
abstract: Two high performance liquid chromatographic methods (HPLC-DAD and LC-MS/MS) were developed to analyze tetracycline (TC) residues in pig meat (pork) samples. The method involved a sample preparation using a solid-liquid extraction (SLE) by McIlvaine buffer, followed by a solid-phase extraction (SPE) clean-up using Strata-XL cartridges. The developed sample clean-up resulted in a selective chromatogram in the HPLC-DAD separation and a reduced matrix effect (ME) in LC-MS/MS analysis. Moreover, HPLC columns packed with core-shell particles were tested for separation, which further enhanced the sensitivity and the selectivity of determinations. The validation of the methods for pig samples was carried out according to European Union 2002/657/EC decision. In addition, validation was also performed for bovine, chicken, and turkey meat samples using HPLC-DAD method. The performance characteristics of determinations were evaluated with both spiked and incurred samples, and were systematically compared. LC-MS/MS technique was found to be more accurate for spiked samples; however, HPLC-DAD method resulted in more reliable concentrations for incurred samples.
authors.affiliation: National Food Chain Safety Office Food and Feed Safety Directorate, Food Toxicological National Reference Laboratory, Mester utca 81, Budapest 1095, Hungary. Electronic address: tolgyesi83@gmail.com.
authors.forename: Ádám
authors.initials: Á
authors.lastname: Tölgyesi
authors.affiliation: Agilent Technologies Sales & Services GmbH und Co. KG, Hewlett-Packard-Strasse 8, Waldbronn 76337, Germany. Electronic address: laszlo.toelgyesi@agilent.com.
authors.forename: László
authors.initials: L
authors.lastname: Tölgyesi
authors.affiliation: National Food Chain Safety Office Food and Feed Safety Directorate, Food Toxicological National Reference Laboratory, Mester utca 81, Budapest 1095, Hungary. Electronic address: pelesek@gmail.com.
authors.forename: Katalin
authors.initials: K
authors.lastname: Békési
authors.affiliation: Chemistry Department, Florida Institute of Technology, 150 West University Boulevard, Melbourne FL 32901, USA. Electronic address: vsharma@fit.edu.
authors.forename: Virender K
authors.initials: VK
authors.lastname: Sharma
authors.affiliation: Budapest University of Technology and Economics, Department of Inorganic and Analytical Chemistry, Szt. Gellért tér 4, Budapest 1111, Hungary. Electronic address: fekete@mail.bme.hu.
authors.forename: Jenő
authors.initials: J
authors.lastname: Fekete
mesh_terms: D000818:Animals; D002851:Chromatography, High Pressure Liquid; D002853:Chromatography, Liquid; D008460:Meat / Q000032:analysis*; D052616:Solid Phase Extraction; D013552:Swine; D053719:Tandem Mass Spectrometry; D013754:Tetracyclines / Q000032:analysis*
chemical_list: D013754:Tetracyclines
keywords: Core–shell HPLC column; HPLC–DAD; LC–MS/MS; Matrix effect; Strata solid-phase extraction; Tetracyclines