首页> 美国卫生研究院文献>International Journal of Analytical Chemistry >Isocratic Resolution of Fluoroquinolone-Based Antibiotics on the Phenylethyl-Bonded Phase under Nonaqueous Elution: A Consideration of the Separation Mechanism
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Isocratic Resolution of Fluoroquinolone-Based Antibiotics on the Phenylethyl-Bonded Phase under Nonaqueous Elution: A Consideration of the Separation Mechanism

机译:非水洗脱下苯乙酮键合相上基于氟喹诺酮类抗生素的等度拆分:对分离机理的考虑

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摘要

This paper reports the isocratic resolution of 10 fluoroquinolone-based antibiotics and their precursors on the phenylethyl-bonded phase under the elution of the nonaqueous mobile phase composed of acetonitrile, methanol, acetic acid, and triethylamine. Most of the analytes were baseline resolved within 10 minutes. The interaction simulation and Fourier-transform infrared spectroscopy (FTIR) data indicated that the carbonyl-containing group, a secondary or tertiary amine of an analyte, was heavily involved in the retention, resulting in retention with residual silanol groups on the stationary phase. In some cases, the elution reversal or resolution enhancement of analytes was observed when the volume of acidic or basic additive in the mobile phase was dominant. However, the π-π complexation interaction between the fluorine-attached phenyl group of the analyte and the phenylethyl moiety on the stationary phase was not observed. Consequently, the resolution could not be reproduced either on the other stationary phase modified with C18, phenyl, or phenylhexyl moiety under the same chromatographic conditions or under the aqueous elution.
机译:本文报道了在由乙腈,甲醇,乙酸和三乙胺组成的非水流动相洗脱下,10种氟喹诺酮类抗生素及其前体在苯乙基键合相上的等度拆分。大多数分析物在10分钟内即可完成基线分离。相互作用模拟和傅立叶变换红外光谱(FTIR)数据表明,分析物的含羰基基团(仲胺或叔胺)大量参与保留,导致保留相上残留的硅烷醇基保留。在某些情况下,当流动相中酸性或碱性添加剂的体积占主导地位时,观察到分析物的洗脱反转或分离度提高。然而,未观察到分析物的附有氟的苯基与固定相上的苯乙基部分之间的π-π络合相互作用。因此,在相同的色谱条件下或在水洗脱条件下,在用C18,苯基或苯基己基部分改性的其他固定相上,均无法获得分离度。

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