Department of Pharmacology, Faculty of Veterinary Medicine, Kasetsart University, Bangkok 10900, Thailand.
Department of Environmental Technology and Management, Faculty of Environment, Kasetsart University, Bangkok 10900, Thailand.
J Food Drug Anal. 2019 Jan;27(1):118-134. doi: 10.1016/j.jfda.2018.06.003. Epub 2018 Jul 3.
A reliable, selective and rapid multiclass method has been developed for the simultaneous determination of 55 antibacterial drug residues in shrimp muscle samples by ultra high performance liquid chromatography-tandem mass spectrometry. The investigated compounds comprise of eight different classes, namely fluoroquinolones, sulfonamides and synergistic agents, tetracyclines, macrolides, lincosamides, penicillins, nitroimidazole and amphenicols. A simple liquid extraction procedure was developed consisting of extraction with a mixture of acetonitrile and ethylenediaminetetraacetic acid (EDTA), followed by a defatting step with n-hexane. Chromatographic conditions were optimized, obtaining a running time <10 min. Mean recoveries ranged from 74.3% to 113.3%. For precision test, relative standard deviations (RSD, %) were lower than 15.0% and 24.0% for repeatability and reproducibility, respectively. Limits of detection and quantification ranged from 1.0 to 5.0 ng/g and 3.0-10.0 ng/g, respectively. Finally, the method was applied to real samples and the results demonstrated that enrofloxacin, ciprofloxacin, pefloxacin and doxycycline were quantifiable in shrimp samples.
已开发出一种可靠、选择性和快速的多类方法，用于通过超高效液相色谱-串联质谱法同时测定虾肌肉样品中 55 种抗菌药物残留。研究的化合物包括 8 个不同的类别，即氟喹诺酮类、磺胺类和增效剂、四环素类、大环内酯类、林可酰胺类、青霉素类、硝基咪唑类和酰胺醇类。建立了一种简单的液液萃取程序，包括用乙腈和乙二胺四乙酸（EDTA）的混合物萃取，然后用正己烷脱脂。优化了色谱条件，运行时间<10 min。平均回收率在 74.3%至 113.3%之间。精密度试验中，重复性和再现性的相对标准偏差（RSD，%）分别低于 15.0%和 24.0%。检测限和定量限分别为 1.0-5.0 ng/g 和 3.0-10.0 ng/g。最后，该方法应用于实际样品，结果表明虾样品中可定量检测恩诺沙星、环丙沙星、培氟沙星和强力霉素。
