Department of Analytical Chemistry, University of Extremadura, Avda. Elvas, S/N, 06071 Badajoz, Spain.
J Chromatogr B Analyt Technol Biomed Life Sci. 2010 Feb 1;878(3-4):398-402. doi: 10.1016/j.jchromb.2009.12.012. Epub 2009 Dec 16.
A selective method based on high-performance liquid chromatography with electrochemical detection (HPLC-ECD) has been developed to enable simultaneous determination of three fluoroquinolones (FQs), namely danofloxacin (DANO), difloxacin (DIFLO) and sarafloxacin (SARA). The fluoroquinolones are separated on a Novapack C-18 column and detected in a high sensitivity amperometric cell at a potential of +0.8 V. Solid-phase extraction was used for the extraction of the analytes in real samples. The range of concentration examined varied from 10 to 150 ng g(-1) for danofloxacin, from 25 to 100 ng g(-1) for sarafloxacin and from 50 to 315 ng g(-1) for difloxacin, respectively. The method presents detection limits under 10 ng g(-1) and recoveries around 90% for the three analytes have been obtained in the experiments with fortified samples. This HPLC-ECD approach can be useful in the routine analysis of antibacterial residues being less expensive and less complicated than other more powerful tools as hyphenated techniques.
建立了一种基于高效液相色谱电化学检测(HPLC-ECD)的选择性方法,可同时测定三种氟喹诺酮类药物(FQs),即达氟沙星(DANO)、二氟沙星(DIFLO)和沙拉沙星(SARA)。氟喹诺酮类药物在 Novapack C-18 柱上分离,并在高灵敏度安培池在+0.8 V 的电位下检测。固相萃取用于从实际样品中提取分析物。浓度检测范围分别为达氟沙星 10-150ng g(-1),沙拉沙星 25-100ng g(-1),二氟沙星 50-315ng g(-1)。该方法的检测限低于 10ng g(-1),在加标样品的实验中,三种分析物的回收率约为 90%。与其他更强大的工具(如联用技术)相比,这种 HPLC-ECD 方法成本更低,操作更简单,可用于常规的抗菌残留分析。