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Validated multiclass targeted determination of antibiotics in fish with high performance liquid chromatography–benchtop quadrupole orbitrap hybrid mass spectrometry
Food Chemistry ( IF 8.5 ) Pub Date : 2018-03-19 , DOI: 10.1016/j.foodchem.2018.03.072
Luca Chiesa , Sara Panseri , Elisa Pasquale , Renato Malandra , Radmila Pavlovic , Francesco Arioli

High performance liquid chromatography, coupled with a benchtop Q-Exactive Orbitrap high-resolution mass spectrometer, was successfully applied for the determination of 24 target antibiotics (selected beta-lactams, tetracyclines, fluoroquinolones, sulfonamids, phenicols, macrolides, cephalosporins, lincosamides, diaminopyrimidine) in fish matrices. The Q-Exactive parameters were carefully studied to accomplish the best compromise between a suitable scan speed and selectivity, considering the restrictions associated with generic sample preparation methodology. Retention time, an exact mass with tolerance of 2 ppm and data-dependent MS2 spectra were the main identifiers. The method was validated through specificity, linearity, recovery, intra- and inter-day repeatability, decision limit (CCα) and detection capability (CCβ), according to 2002/657/EC. The values of CCα and CCβ ranged from 29.2 to 36.8 and 32.5 to 48.9, respectively, while overall recovery ranged from 91.1 to 105.6%. Fifty fish samples were analysed, showing the sporadic incidence of enrofloxacin, chlortetracycline, oxytetracycline, amoxicillin and trimethoprim, albeit below the maximum residual levels.



中文翻译:

高效液相色谱-台式四极杆Orbitrap混合质谱法对鱼类中的抗生素进行多目标验证

高效液相色谱仪与台式Q-Exactive Orbitrap高分辨率质谱仪相结合,已成功用于测定24种目标抗生素(选定的β-内酰胺,四环素,氟喹诺酮类,磺胺类,酚类,大环内酯类,头孢菌素,林可酰胺,二氨基嘧啶)在鱼基质中。考虑到通用样品制备方法的局限性,对Q-Exactive参数进行了仔细研究,以在合适的扫描速度和选择性之间实现最佳折衷。保留时间,精确的质量(公差为2 ppm)和取决于数据的MS 2光谱是主要的识别符。根据2002/657 / EC,该方法通过特异性,线性,回收率,日内和日间重复性,决策极限(CCα)和检测能力(CCβ)进行了验证。CCα和CCβ值的范围分别为29.2至36.8和32.5至48.9,而总回收率的范围为91.1至105.6%。分析了五十个鱼样品,显示了恩诺沙星,金霉素,土霉素,阿莫西林和甲氧苄氨辛酯的零星发生率,尽管低于最大残留水平。

更新日期:2018-03-19
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