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, v/v) 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.

中文翻译：

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UPLC结合双通道荧光检测法同时测定禽蛋中的四环素和氟喹诺酮类药物

建立了一种采用超高效液相色谱-荧光检测（UPLC-FLD）同时测定家禽鸡蛋中三种四环素（土霉素、四环素和多西环素）和两种氟喹诺酮类（环丙沙星和恩诺沙星）残留的创新、快速、稳定的方法，并优化。将样品均质并用乙腈/超纯水 (90:10, v/v)，然后通过固相萃取 (SPE) 进行纯化。在ACQUITY UPLC BEH C18色谱柱（1.7 µm，2.1 mm × 100 mm）上实现LC分离，流动相由乙腈和0.1 mol/L含50 mmol/L氯化镁的丙二酸溶液组成（pH为用氨水调节至 5.5）。当五种目标药物在定量限、0.5 倍最大残留限量 (MRL)、1.0 MRL 和 2.0 MRL 下加标时，回收率均在 83.5% 以上，精密度在 1.99% 至 6.24% 之间。这些品质因数符合欧盟和美国 FDA 的参数验证规定。目标的检测限和定量限分别为 0.1–13.4 µg/kg 和 0.3–40.1 µg/kg。所提出的方法很容易扩展到85个鸡蛋样品中目标药物残留的定量分析，