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Ionic liquids as mobile phase additives for the high-performance liquid chromatographic analysis of fluoroquinolone antibiotics in water samples

机译:离子液体作为流动相添加剂,用于高效液相色谱分析水中的氟喹诺酮类抗生素

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In this work, four ionic liquids differing in the length of the alkyl chain on the imidazolium cation and one ionic liquid containing tetraethylammonium, all with the same counterion, (i.e. 1-ethyl-3-methylimidazolium tetrafluoroborate (EMIm-BF4), 1-butyl-3-methylimidazolium tetrafluoroborate (BMIm-BF4), 1-hexyl-3-methylimidazolium tetrafluoroborate (HMIm-BF4), 1-methyl-3-octylimidazolium tetrafluoroborate (MOIm-BF4), and tetraethylammonium tetrafluroborate (Et4N-BF4)) were tested as mobile phase additives for HPLC separation of a group of seven basic fluoroquinolone (FQ) antibiotics for human and veterinary use (i.e. fleroxacin, ciprofloxacin, lomefloxacin, danofloxacin, enrofloxacin, sarafloxacin, and difloxacin) using a conventional reversed-phase Nova-Pak C-18 Column. Fluorescence detection was used. Among the ionic liquids selected, use of BMIm-BF4 enabled effective separation of these compounds with relatively low analysis time (14 min). The best separation was achieved by isocratic elution at 1 mL min(-1) with 5 mmol L-1 BMIm-BF4 and 10 mmol L-1 ammonium acetate at pH 3.0 with 13% (v/v) acetonitrile. Limits of detection (LODs) for fluorescence detection were in the range 0.5-11 mu g L-1. The method was tested by analyzing several water samples after the optimization of a suitable solid-phase extraction (SPE) procedure using Oasis HLB cartridges. Mean recovery values were above 84% for all analytes with LODs in the range 1-29 ng L-1.
机译:在这项工作中,四种咪唑阳离子上烷基链长度不同的离子液体和一种含有四乙基铵的离子液体,所有离子液体都具有相同的抗衡离子(即1-乙基-3-甲基咪唑四氟硼酸酯(EMIm-BF4),1-分别是3-甲基咪唑四氟硼酸酯(BMIm-BF4),1-己基-3-甲基咪唑四氟硼酸酯(HMIm-BF4),1-甲基-3-辛咪唑四氟硼酸酯(MOIm-BF4)和四乙基四氟硼酸铵(Et4N-BF4))。经过测试,用作流动相添加剂,使用常规反相Nova-反相色谱法,用于HPLC分离用于人和兽用的七种基本氟喹诺酮(FQ)抗生素(即氟罗沙星,环丙沙星,洛美沙星,达诺氟沙星,恩诺沙星,萨拉罗沙星和地氟沙星) C-18柱。使用荧光检测。在所选的离子液体中,使用BMIm-BF4能够以相对较低的分析时间(14分钟)有效分离这些化合物。最佳分离是通过在5 mL L-1 BMIm-BF4和10 mmol L-1乙酸铵在pH 3.0和1%(v / v)乙腈的1 mL min(-1)下进行等度洗脱实现的。荧光检测的检测限(LOD)在0.5-11μg L-1范围内。在使用Oasis HLB滤芯优化合适的固相萃取(SPE)程序后,通过分析几个水样来测试该方法。对于所有LOD在1-29 ng L-1范围内的分析物,平均回收率均高于84%。

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