Nozal Nalda María Jesús, Bernal Yagüe José Luis, Gómez María Teresa Martín, Jiménez Sevilla Juan José, Bernal del Nozal José, Higes Pascual Mariano
Department of Analytical Chemistry, Faculty of Sciences, University of Valladolid, Spain.
J Sep Sci. 2006 Feb;29(3):405-13. doi: 10.1002/jssc.200500423.
A new LC-ESI-MS method was developed for the determination of residues of the antibacterial tylosins A, B, C and D in honey. The procedure employed an SPE on polymeric cartridges for the isolation of tylosins from diluted honey. Chromatographic separation of the tylosins was performed on a C18 column (150 x 4.60 mm2 ID, 5 microm) using a ternary gradient made of formic acid 1% in water (solvent A), methanol (solvent B) and ACN (solvent C) as mobile phase, at 30 degrees C and at a flow rate of 0.8 mL/min. Average analyte recoveries for the studied compounds ranged from 89 to 106% in replica sets of fortified honey samples. The detection limits for the four drugs studied were between 2 and 3 microg/kg. The developed method has been applied to the analysis of tylosin residues in honey from veterinarian treated beehives fed with the technical product, which contains the four compounds and is a new candidate antibiotic to treat American foulbrood disease of honey bee colonies.
开发了一种新的液相色谱 - 电喷雾电离质谱（LC - ESI - MS）方法，用于测定蜂蜜中抗菌泰乐菌素A、B、C和D的残留量。该方法采用聚合物柱固相萃取（SPE）从稀释的蜂蜜中分离泰乐菌素。泰乐菌素的色谱分离在C18柱（内径150×4.60 mm²，粒径5微米）上进行，以1%甲酸水溶液（溶剂A）、甲醇（溶剂B）和乙腈（溶剂C）组成的三元梯度溶液为流动相，柱温30℃，流速0.8 mL/min。在所研究的加标蜂蜜样品复样中，所研究化合物的平均分析物回收率在89%至106%之间。所研究的四种药物的检测限在2至3微克/千克之间。所开发的方法已应用于分析来自用含有这四种化合物的工业产品喂养的、经兽医处理的蜂箱所产蜂蜜中的泰乐菌素残留量，该工业产品是治疗蜜蜂群体美洲幼虫腐臭病的一种新型候选抗生素。
