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Ultra-high performance liquid chromatography with fluorescence detection following salting-out assisted liquid–liquid extraction for the analysis of benzimidazole residues in farm fish samples
Journal of Chromatography A ( IF 4.1 ) Pub Date : 2018-02-21 , DOI: 10.1016/j.chroma.2018.02.042
Carmen Tejada-Casado , Francisco J. Lara , Ana M. García-Campaña , Monsalud del Olmo-Iruela

Ultra-high performance liquid chromatography (UHPLC) coupled with fluorescence detection (FL) has been proposed for the first time to determine thirteen benzimidazoles (BZs) in farmed fish samples. In order to optimize the chromatographic separation, parameters such as mobile phase composition and flow rate were carefully studied, establishing a gradient mode with a mobile phase consisted of water (solvent A) and acetonitrile (solvent B) at a flow rate of 0.4 mL/min. The separation was performed on a Zorbax Eclipse Plus RRHD C18 column (50 × 2.1 mm, 1.8 μm), involving a total analysis time lower than 12 min. Salting-out assisted liquid-liquid extraction (SALLE) was applied as sample treatment to different types of farmed fish (trout, sea bream and sea bass). To obtain satisfactory extraction efficiencies for the studied analytes, several parameters affecting the SALLE procedure were optimized including the amount of sample, type and volume of the extraction solvent, and the nature and amount of the salt used. Characterization of the method in terms of performance characteristics was carried out, obtaining satisfactory results for the linearity (R2 ≥ 0.997), repeatability (RSD ≤ 6.1%), reproducibility (RSD ≤ 10.8%) and recoveries (R ≥ 79%; RSD ≤ 7.8%). Detection limits between 0.04–29.9 μg kg−1 were obtained, demonstrating the applicability of this fast, simple and environmentally friendly method.



中文翻译:

超高效液相色谱法,在盐析辅助液液萃取后进行荧光检测,用于分析养殖鱼类样品中的苯并咪唑残留量

首次提出了将超高效液相色谱(UHPLC)与荧光检测(FL)结合使用的方法,用于测定养殖鱼类样品中的十三种苯并咪唑(BZs)。为了优化色谱分离效果,对流动相组成和流速等参数进行了仔细研究,建立了由水(溶剂A)和乙腈(溶剂B)组成的流动相(流速为0.4 mL / mL)组成的梯度模式。分钟 分离是在Zorbax Eclipse Plus RRHD C 18上进行的色谱柱(50×2.1 mm,1.8μm),总分析时间少于12分钟。盐析辅助液-液萃取(SALLE)作为样品处理应用于不同类型的养殖鱼(鳟鱼,鲷鱼和鲈鱼)。为使研究的分析物获得满意的萃取效率,对影响SALLE程序的几个参数进行了优化,包括样品量,萃取溶剂的类型和体积以及所用盐的性质和量。在性能特征方面的方法的特征进行,获得满意的结果为线性(R 2  ≥0.997),重复性(RSD≤6.1%),重现性(RSD≤10.8%)和回收率(R≥79%; RSD ≤7.8%)。检出限在0.04–29.9μgkg -1之间 获得了该方法,证明了这种快速,简单和环保的方法的适用性。

更新日期:2018-02-21
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