Department of Chemistry and Physics (Analytical Chemistry Area), Research Centre for Agricultural and Food Biotechnology (BITAL), University of Almerı́a, Agrifood Campus of International Excellence, Almerı́a, Spain.
J Agric Food Chem. 2013 Jan 30;61(4):829-39. doi: 10.1021/jf3048498. Epub 2013 Jan 16.
A simple and rapid method is described for the determination of veterinary drug (VD) residues in honey samples using turbulent flow chromatography coupled to ultrahigh-performance liquid chromatography-Orbitrap mass spectrometry (TFC-UHPLC-Orbitrap-MS). Honey samples were diluted with an aqueous solution of Na(2)EDTA (0.1 M). Then, they were injected into the chromatographic system including a TFC column. Afterward, the analytes were transferred to an UHPLC analytical column, where they were determined by UHPLC-Orbitrap-MS. Mean recoveries were obtained at three concentration levels (5, 10, and 50 μg/kg), ranging from 68 to 121% for most compounds. Repeatability (intraday precision) and interday precision (expressed as relative standard deviation, RSD) were <25% for most compounds. Limits of quantification (LOQs) ranged from 5 to 50 μg/kg and limits of identification (LOIs) from 0.1 to 50 μg/kg. The developed method was applied in honey samples, and it was fast and nonlaborious.
本文描述了一种使用湍流流色谱-超高液相色谱-轨道阱质谱(TFC-UHPLC-Orbitrap-MS)测定蜂蜜样品中兽药(VD)残留量的简单、快速方法。蜂蜜样品用 0.1 M 的 Na(2)EDTA 水溶液稀释。然后,将其注入包括 TFC 柱的色谱系统。之后,分析物被转移到 UHPLC 分析柱上,通过 UHPLC-Orbitrap-MS 进行测定。在三个浓度水平(5、10 和 50 μg/kg)下,大多数化合物的平均回收率在 68%至 121%之间。大多数化合物的日内精密度(重复性)和日间精密度(相对标准偏差,RSD)均<25%。定量限(LOQs)范围为 5 至 50 μg/kg,鉴定限(LOIs)范围为 0.1 至 50 μg/kg。该方法已应用于蜂蜜样品的测定,具有快速、非劳动密集型的特点。