Simultaneous Determination of Nine Sulphonamides by LC-MS for Routine Control of Raw Honey Samples
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Simultaneous Determination of Nine Sulphonamides by LC-MS for Routine Control of Raw Honey Samples Isabel Guillén 1 & Lucía Guardiola 1 & Luis Almela 2 & Estrella Núñez-Delicado 1 & Jose A. Gabaldón 1
Received: 29 July 2016 / Accepted: 13 October 2016 # Springer Science+Business Media New York 2016
Abstract A liquid chromatography-mass spectrometry method for the simultaneous determination of nine sulphonamides (sulphadiazine, sulphathiazole, sulphapyridine, sulphamerazine, sulphamethizole, sulphasoxazole, sulphamethoxypyridazine, sulphamethoxazole and sulphadimethoxine) in honey samples was developed. Sample pretreatment included acidic hydrolysis, followed by solid-phase extraction on a Sep-Pack® C18. Separation is carried out in a C18 column and mobile phases consisting of acetic acid/methanol mixtures. Detection is performed by mass spectrometry with ion trap, using electrospray interface in the positive ionization mode. Method validation has been performed according to European Commission Decision 2002/657/EC criteria, in terms of linearity, trueness, precision, specificity, decision limit (CCα) and detection capability (CCβ). Linearity was obtained with an average coefficient of determination (R2) higher than 0.9995 in matrix. Typical recoveries in fortified honey samples ranged between 89 and 118 % at all levels tested (5, 10, 50 and 100 μg/kg). The method demonstrated good intra- and interbatch precision and accuracy. No interferences with the peaks of interest were observed throughout the chromatographic run. The method has been successfully applied to the analysis of raw honey samples. Forty-five (21 %) of 215 analysed were positive (range 6.7–140.8 μg/kg) for sulphonamides.
* Jose A. Gabaldón [email protected] 1
Department of Food Technology and Nutrition, San Anthony Catholic University of Murcia, Avenida de los Jerónimos s/n, 30107 Murcia, Guadalupe, Spain
2
Department of Agricultural Chemistry, University of Murcia, Campus of Espinardo, 30100 Murcia, Spain
Keywords Drug residues . Sulphonamides . LC-MS . Honey . Commission decision 2002/657/EC
Introduction Over the last decades, food production systems have evolved from small farming units to large-scale intensive farming operations. As a consequence of such evolution, veterinary drugs have been increasingly used for the treatment of bacterial diseases in animals, fish and plants to control, prevent, or treat infection diseases and to enhance animal growth and feed efficiency (Tollefson and Miller 2000). As a result of their widespread use, residues of sulphonamides were found in animal products for human consumption such as milk, eggs, fish, meat and honey (Hoopingarner and Nelson 1988). In fact, since the 1990s, there has been an increase in the number of cases related with contamination of natural honey with residues of sulphonamides, used in apiculture for the treatment of bacterial diseases like American and European foulbrood (Spivak 2000; Waite et al. 2003). Sulphonamides are relatively stable chemotherapeutics to control a number of
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