Nozal M J, Bernal J L, Martín M T, Jiménez J J, Bernal J, Higes M
Department of Analytical Chemistry, Faculty of Sciences, University of Valladolid, 47005 Valladolid, Spain.
J Chromatogr A. 2006 May 26;1116(1-2):102-8. doi: 10.1016/j.chroma.2006.03.028. Epub 2006 Mar 30.
A liquid chromatography with diode array or electrospray ionisation mass spectrometry detection (LC-DAD-ESI-MS) method for the determination of tiamulin residues in honey is presented. The procedure employs a solid-phase extraction (SPE) on polymeric cartridges for the isolation of tiamulin from honey samples diluted in aqueous solution of tartaric acid. Chromatographic separation of the tiamulin is performed, in isocratic mode, on a C18 column using methanol and ammonium carbonate 0.1% in water, in proportion (30:70, v/v). Average analyte recoveries were from 88 to 106% in replica sets of fortified honey samples. The LC-ESI-MS method detection limits differ from 0.5 microg kg(-1) for clear honeys to 1.2 microg kg(-1) for dark honeys. The developed method has been applied to the analysis of tiamulin residues in multifloral honey samples collected from veterinary treated beehives.
本文介绍了一种采用二极管阵列液相色谱或电喷雾电离质谱检测（LC-DAD-ESI-MS）法测定蜂蜜中泰妙菌素残留量的方法。该方法采用聚合物柱进行固相萃取（SPE），从用酒石酸水溶液稀释的蜂蜜样品中分离泰妙菌素。泰妙菌素的色谱分离在等度模式下，于C18柱上进行，流动相为甲醇和0.1%碳酸铵水溶液，比例为（30:70，v/v）。在添加了泰妙菌素的蜂蜜样品重复测定中，平均回收率为88%至106%。LC-ESI-MS法的检测限，清澈蜂蜜为0.5 μg kg⁻¹，深色蜂蜜为1.2 μg kg⁻¹。所建立的方法已应用于分析从经过兽医治疗的蜂箱采集的多花蜂蜜样品中的泰妙菌素残留量。
