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首页> 外文期刊>RSC Advances >Simultaneous determination of selected veterinary antibiotics in Nile tilapia (Orechromis niloticus) and water samples by HPLC/UV and LC-MS/MS
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Simultaneous determination of selected veterinary antibiotics in Nile tilapia (Orechromis niloticus) and water samples by HPLC/UV and LC-MS/MS

机译：HPLC / UV和LC-MS / MS同时测定尼罗罗非鱼（ Orechromis niloticus ）和水样中的所选兽用抗生素

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摘要

A method was optimized and validated for simultaneous estimation of some antibiotics such as chlortetracycline (CTC), doxycycline (DOX), florfenicol (FF), flumequine (FLU), nalidixic acid (NAL), sulfadiazine (SDI), sulfathiazole (STZ) and trimethoprim (TMP) in fish muscle and water samples. The method is based on solid phase extraction (SPE) and simple extraction followed by high performance liquid chromatography with ultraviolet detection (HPLC-UV). The HPLC method was optimized using experimental design. The optimum conditions for separation determined with the aid of central composite design were: (1) initial mobile phase concentration: 0.1% formic acid in water/acetonitrile (90/10, v/v), (2) column temperature 25 °C and (3) mobile phase flow rate (1.2 ml min?1). The optimized method was validated according to ICH guidelines. The detection and quantification limits were between 0.2–0.4 and 0.3–0.6 μg kg?1, respectively, for fish and between 0.005–0.02 and 0.01–0.08 μg ml?1, respectively, for water. The procedure was also applied to the analysis of spiked Nile tilapia samples. Three antibiotics (SDI, CTC and FF) were orally administered and the residue was analyzed using liquid chromatography-electro spray ionization-mass spectrometry with positive ion mode (LC-ESI/MS).
机译：优化并验证了一种方法，用于同时估算某些抗生素，例如金霉素（CTC），多西环素（DOX），氟苯尼考（FF），氟米汀（FLU），萘啶酸（NAL），磺胺嘧啶（SDI），磺胺噻唑（STZ）和鱼肌肉和水样品中的甲氧苄啶（TMP）。该方法基于固相萃取（SPE）和简单萃取，然后进行高效液相色谱和紫外检测（HPLC-UV）。使用实验设计优化了HPLC方法。借助中心复合设计确定的最佳分离条件为：（1）初始流动相浓度：水/乙腈（90/10，v / v）中的0.1％甲酸，（2）柱温25°C和（3）流动相流速（1.2 ml min ？1 ）。根据ICH指南验证了优化方法。鱼类的检出限和定量限分别为0.2–0.4至0.3–0.6μgkg ？1 ，0.005–0.02至0.01–0.08μgml ？1 分别代表水。该方法还应用于加标尼罗罗非鱼样品的分析。口服施用了三种抗生素（SDI，CTC和FF），并使用液相色谱-电喷雾电离质谱以正离子模式（LC-ESI / MS）分析了残留物。

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