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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:通过HPLC / UV和LC-MS / MS同时测定尼罗替尼亚(OreChromis Niloticus)和水样中所选兽医抗生素的测定

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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 degrees 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 mu g kg(-1), respectively, for fish and between 0.005-0.02 and 0.01-0.08 mu g 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:优化和验证了一种方法,同时估计一些抗生素,如氯化酰胞嘧啶(CTC),十二酸盐(DOX),氟芬糖(FF),FLUMEQUINE(FLU),萘啶酸(NAL),磺胺酰胺(SDI),磺胺唑(STZ)和Trimethokim(TMP)在鱼肌和水样中。该方法基于固相萃取(SPE)和简单提取,然后具有高效液相色谱,具有紫外检测(HPLC-UV)。使用实验设计优化了HPLC方法。借助中央复合设计确定的最佳条件是:(1)初始流动相浓度:水/乙腈(90/10,v / v)中0.1%甲酸(90/10,v / v),(2)柱温度25℃和(3)流动相流速(1.2mL min(-1))。根据ICH指南验证了优化的方法。检测和定量限制分别为鱼类和0.005-0.02和0.01-0.08μg(-10.0.08μg(-1)的0.2-0.4和0.3-0.6μgkg(-1)。该程序也适用于分析掺入尼罗罗非鱼样品。口服施用三种抗生素(SDI,CTC和FF),使用液相色谱 - 电离电离质谱法用阳性离子模式(LC-ESI / MS)分析残余物。

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  • 来源
    《RSC Advances》 |2017年第73期|共12页
  • 作者单位

    Suez Canal Univ Dept Pharmaceut Analyt Chem Fac Pharm Ismailia 41522 Egypt;

    Suez Canal Univ Dept Pharmaceut Analyt Chem Fac Pharm Ismailia 41522 Egypt;

    Suez Canal Univ Dept Pharmaceut Analyt Chem Fac Pharm Ismailia 41522 Egypt;

    Suez Canal Univ Dept Fish Dis &

    Management Fac Vet Med Ismailia Egypt;

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  • 原文格式 PDF
  • 正文语种 eng
  • 中图分类 化学;
  • 关键词

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