Department of Analytical Chemistry, Faculty of Sciences, Campus Fuentenueva, s/n, E-18071 Granada, Spain.
Talanta. 2012 May 15;93:193-9. doi: 10.1016/j.talanta.2012.02.011. Epub 2012 Feb 28.
A reliable and rapid ultra high performance liquid chromatography tandem mass spectrometry (UHPLC-MS/MS) method has been developed for the determination of the eight quinolones of veterinary use regulated by European Union (marbofloxacin, ciprofloxacin, danofloxacin, enrofloxacin, sarafloxacin, difloxacin, flumequine and oxolinic acid). Chromatographic conditions were optimized in order to increase sample throughput and sensitivity. The antibiotics were detected by electrospray ionization in positive ion mode with multiple reaction monitoring (MRM) and MS/MS conditions were optimized in order to increase selectivity, selecting the corresponding product ions for quantification and identification. The separation was achieved in 3 min, using a Zorbax Eclipse Plus C18 column (50 mm × 2.1mm, 1.8 μm), with a mobile phase of 0.02% aqueous formic acid solution and acetonitrile. A dispersive solid phase extraction methodology, often referred to as the "QuEChERS" (quick, easy, cheap, effective, rugged, and safe) method, was optimized for extraction of the quinolones from honey and also it was evaluated for other bee products such as royal jelly and propolis. The method was validated for each matrix in terms of linearity, trueness, precision, limits of detection (LODs) and quantification (LOQ). LODs ranged between 0.2 and 4.1 μg kg(-1) with precision lower than 12% and satisfactory recoveries in most cases. The method was also applied for studying the occurrence of these antibiotics in several market samples.
已经开发出一种可靠且快速的超高效液相色谱串联质谱（UHPLC-MS/MS）方法，用于测定受欧盟监管的八种兽用喹诺酮类药物（马波沙星、环丙沙星、丹诺沙星、恩诺沙星、沙拉沙星、二氟沙星、氟甲喹和恶喹酸）。优化了色谱条件，以提高样品通量和灵敏度。抗生素通过电喷雾电离在正离子模式下检测，采用多重反应监测（MRM），并优化了 MS/MS 条件，以提高选择性，选择相应的产物离子进行定量和鉴定。在 3 分钟内，使用 Zorbax Eclipse Plus C18 柱（50mm×2.1mm，1.8μm），以 0.02%水甲酸溶液和乙腈作为流动相，实现了分离。优化了分散固相萃取方法，通常称为“QuEChERS”（快速、简便、廉价、有效、耐用、安全）方法，用于从蜂蜜中提取喹诺酮类药物，并对其他蜂产品，如蜂王浆和蜂胶进行了评估。该方法在每个基质中均进行了线性、准确度、精密度、检测限（LOD）和定量限（LOQ）的验证。LOD 范围在 0.2 至 4.1μgkg(-1)之间，精密度低于 12%，在大多数情况下回收率令人满意。该方法还应用于研究这些抗生素在几种市场样品中的存在情况。
