College of Animal Science and Technology, Yangzhou University, Yangzhou 225009, China.
Joint International Research Laboratory of Agriculture & Agri-Product Safety, Yangzhou University, Yangzhou 225009, China.
Molecules. 2021 Sep 19;26(18):5684. doi: 10.3390/molecules26185684.
An innovative, rapid and stable method for simultaneous determination of three tetracycline (oxytetracycline, tetracycline and doxycycline) and two fluoroquinolone (ciprofloxacin and enrofloxacin) residues in poultry eggs by ultra-high performance liquid chromatography-fluorescence detection (UPLC-FLD) was established and optimized. The samples were homogenized and extracted with acetonitrile/ultrapure water (90:10, ) and then purified by solid-phase extraction (SPE). LC separation was achieved on an ACQUITY UPLC BEH C18 column (1.7 µm, 2.1 mm × 100 mm), and the mobile phase was composed of acetonitrile and a 0.1 mol/L malonic acid solution containing 50 mmol/L magnesium chloride (the pH was adjusted to 5.5 with ammonia). When the five target drugs were spiked at the limit of quantification, 0.5 times the maximum residue limit (MRL), 1.0 MRL and 2.0 MRL, the recoveries were above 83.5% and the precision ranged from 1.99% to 6.24%. These figures of merit complied with the parameter validation regulations of the EU and U.S. FDA. The limits of detection and quantifications of the targets were 0.1-13.4 µg/kg and 0.3-40.1 µg/kg, respectively. The proposed method was easily extended to quantitative analyses of target drug residues in 85 egg samples, thus demonstrating its reliability and applicability.
建立并优化了一种超高效液相色谱-荧光检测法（UPLC-FLD），用于同时检测家禽蛋中三种四环素（土霉素、四环素和强力霉素）和两种氟喹诺酮（环丙沙星和恩诺沙星）残留的创新、快速、稳定的方法。样品用乙腈/超纯水（90:10，）匀浆提取，然后通过固相萃取（SPE）进行纯化。LC 分离在 ACQUITY UPLC BEH C18 柱（1.7 µm，2.1 mm × 100 mm）上进行，流动相由乙腈和含有 50 mmol/L 氯化镁的 0.1 mol/L 丙二酸溶液组成（用氨水调节 pH 值至 5.5）。当五种目标药物在限量、0.5 倍最大残留限量（MRL）、1.0 MRL 和 2.0 MRL 时进行加标，回收率均在 83.5%以上，精密度在 1.99%至 6.24%之间。这些衡量指标符合欧盟和美国 FDA 的参数验证法规。目标物的检测限和定量限分别为 0.1-13.4 µg/kg 和 0.3-40.1 µg/kg。该方法易于扩展到 85 个鸡蛋样品中目标药物残留的定量分析，因此证明了其可靠性和适用性。
