Abstract

In this work, a porous polyvinylpyrrolidone/single-walled carbon nanotube incorporated polymerized high internal phase emulsion (PVP/SWCNT-polyHIPE) monolithic column was fabricated and developed as a solid phase extraction (SPE) adsorbent coupled with high performance liquid chromatography-fluorescence detection (SPE-HPLC-FLD) for the determination of tetracycline (TC), oxytetracycline (OTC), chlorotetracycline (CTC), and doxycycline (DC) in environmental water samples. The proposed monolithic sorbent was easily produced by in-situ polymerizing of high internal phase emulsions (HIPEs), and performed high extraction ability to the four tetracycline antibiotics (TCs). The extraction conditions including sample pH, sample flow rate, sample volume, desorption solvent and its volume were studied by investigating the recoveries of the four TCs, and the optimal extraction conditions were obtained. Under the optimized conditions, the PVP/SWCNT-polyHIPE based SPE-HPLC-FLD method exhibited good linearity in the range of 20–800 ng/mL for four tetracycline antibiotics with correlation coefficients higher than 0.9996. For water samples, the detection limits (LODs, S/N = 3) ranged from 1.0–2.5 ng mL⁻¹ for four tetracycline antibiotics. The intra-day (n = 15) and inter-day (n = 5) precisions (expressed in terms of relative standard deviation (RSD %) were in the range of 0.5–2.2 and 1.3–5.7%, respectively. The spiked recoveries were in the range of 85.0–101.7 % with RSDs lower than 4.0%. Furthermore, the prepared polyHIPE monoliths allowed more than 100 extraction cycles without any loss in the extraction efficiency. The developed method enables us to detect trace tetracycline antibiotics in water samples. The method can be useful in the extraction and determination of antibiotics in all kinds of environmental water samples.

中文翻译：

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聚乙烯吡咯烷酮/单壁碳纳米管掺入 Polyhipe 整料后采用高效液相色谱法测定水样中的四环素类抗生素

摘要

在这项工作中，制备并开发了一种多孔聚乙烯吡咯烷酮/单壁碳纳米管结合聚合高内相乳液（PVP/SWCNT-polyHIPE）整体柱作为固相萃取（SPE）吸附剂与高效液相色谱-荧光检测相结合。 (SPE-HPLC-FLD) 用于测定环境水样中的四环素 (TC)、土霉素 (OTC)、金霉素 (CTC) 和强力霉素 (DC)。所提出的整体吸附剂很容易通过高内相乳液（HIPEs）的原位聚合制备，并对四种四环素类抗生素（TCs）具有高萃取能力。通过考察四种 TC 的回收率，研究了样品 pH 值、样品流速、样品体积、解吸溶剂及其体积等萃取条件，并得到最佳提取条件。在优化条件下，基于 PVP/SWCNT-polyHIPE 的 SPE-HPLC-FLD 方法对四种四环素类抗生素在 20-800 ng/mL 范围内表现出良好的线性，相关系数高于 0.9996。对于水样，检测限 (LODs, S/N = 3) 范围为 1.0–2.5 ng mL^-1表示四种四环素抗生素。日内 ( n = 15) 和日间 ( n = 5) 精度（以相对标准偏差 (RSD %) 表示）分别在 0.5-2.2 和 1.3-5.7% 的范围内。加标回收率在 85.0-101.7% 的范围内，RSD 低于 4.0%。此外，制备的 polyHIPE 整体允许超过 100 次提取循环，而提取效率没有任何损失。所开发的方法使我们能够检测水样中的痕量四环素抗生素。该方法可用于各种环境水样中抗生素的提取和测定。