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一种全自动泡腾辅助的基于可切换溶剂的液相微萃取方法:液相色谱法测定人尿液样本中的氧氟沙星。

A fully automated effervescence-assisted switchable solvent-based liquid phase microextraction procedure: Liquid chromatographic determination of ofloxacin in human urine samples.

作者信息

Vakh Christina, Pochivalov Aleksei, Andruch Vasil, Moskvin Leonid, Bulatov Andrey

机构信息

Department of Analytical Chemistry, Institute of Chemistry, Saint-Petersburg University St.Petersburg State University, SPbSU, SPbU, 7/9 Universitetskaya nab., St. Petersburg, 199034 Russia.

Department of Analytical Chemistry, Institute of Chemistry, Saint-Petersburg University St.Petersburg State University, SPbSU, SPbU, 7/9 Universitetskaya nab., St. Petersburg, 199034 Russia.

出版信息

Anal Chim Acta. 2016 Feb 11;907:54-9. doi: 10.1016/j.aca.2015.12.004. Epub 2015 Dec 17.

Abstract

A novel fully automated effervescence-assisted switchable solvent-based liquid phase microextraction procedure has been suggested. In this extraction method, medium-chain saturated fatty acids were investigated as switchable hydrophilicity solvents. The conversion of fatty acid into hydrophilic form was carried out in the presence of sodium carbonate. The injection of sulfuric acid into the solution decreased the pH value of the solution, thus, microdroplets of the fatty acid were generated. Carbon dioxide bubbles were generated in-situ, and promoted the extraction process and final phase separation. The performance of the suggested approach was demonstrated by the determination of ofloxacin in human urine samples using high-performance liquid chromatography with fluorescence detection. This analytical task was used as a proof-of-concept example. Under the optimal conditions, the detector response of ofloxacin was linear in the concentration ranges of 3·10(-8)-3·10(-6) mol L(-1). The limit of detection, calculated from a blank test based on 3σ, was 1·10(-8) mol L(-1). The results demonstrated that the presented approach is highly cost-effective, simple, rapid and environmentally friendly.

摘要

一种新型的全自动泡腾辅助可切换溶剂基液相微萃取方法已被提出。在这种萃取方法中,中链饱和脂肪酸被研究作为可切换亲水性溶剂。脂肪酸向亲水性形式的转化是在碳酸钠存在下进行的。向溶液中注入硫酸会降低溶液的pH值,从而产生脂肪酸微滴。原位产生二氧化碳气泡,促进了萃取过程和最终的相分离。通过使用高效液相色谱荧光检测法测定人尿样中的氧氟沙星,证明了所建议方法的性能。这项分析任务被用作概念验证示例。在最佳条件下,氧氟沙星的检测器响应在3·10(-8)-3·10(-6) mol L(-1)浓度范围内呈线性。基于3σ的空白试验计算出的检测限为1·10(-8) mol L(-1)。结果表明,所提出的方法具有高成本效益、简单、快速且环保的特点。

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