Pantůčková Pavla, Kubáň Pavel
Institute of Analytical Chemistry of the Czech Academy of Sciences, v. v. i., Veveří 97, CZ-60200 Brno, Czech Republic.
Institute of Analytical Chemistry of the Czech Academy of Sciences, v. v. i., Veveří 97, CZ-60200 Brno, Czech Republic.
J Chromatogr A. 2017 Oct 13;1519:137-144. doi: 10.1016/j.chroma.2017.08.084. Epub 2017 Sep 7.
Simultaneous extraction of basic and acidic drugs across thin supported liquid membrane (SLM) and direct injection of the extracted drugs from SLM surface into capillary electrophoresis (CE) were demonstrated. A microextraction device compatible with injection system of commercial CE instrument was filled with 20μL of sample and 10μL of acceptor solution, which were interspaced by the SLM impregnated with 5μL of organic solvent. Extractions of three basic drugs (nortriptyline, haloperidol and loperamide) and two acidic drugs (ketoprofen and naproxen) were achieved at optimized conditions including 1-ethyl-2-nitrobenzene as SLM solvent, natural pH of sample solution, 2.5mM NaOH acceptor solution and 30min extraction time. The extracted drugs were directly injected into CE for separation and quantification in a background electrolyte solution consisting of 30mM ammonium acetate adjusted to pH 4.2 with acetic acid. The entire analytical procedure including drugs extraction, injection, separation and quantification was automated in the CE instrument and the only manual procedures were SLM impregnation and filling the microextraction device with sample and acceptor solutions. The analytical method was suitable for simultaneous determination of basic and acidic drugs in undiluted human urine samples and was used for direct determination of naproxen in urine after oral administration of Nalgesin S tablet. Efficient elimination of sample matrix and selective transfer of basic and acidic drugs were achieved and the hyphenated SLM-CE method was characterized by repeatability of peak areas ranging from 3.7 to 13.4%, linear relationship between peak areas and concentrations (r=0.994-0.999) and limits of detection between 0.05 and 1.5μg/mL.
本文展示了通过薄支撑液膜（SLM）同时萃取碱性和酸性药物，并将从SLM表面萃取的药物直接注入毛细管电泳（CE）的方法。一种与商用CE仪器进样系统兼容的微萃取装置，装有20μL样品和10μL接受液，两者之间由浸渍有5μL有机溶剂的SLM隔开。在优化条件下实现了三种碱性药物（去甲替林、氟哌啶醇和洛哌丁胺）和两种酸性药物（酮洛芬和萘普生）的萃取，优化条件包括以1-乙基-2-硝基苯为SLM溶剂、样品溶液的自然pH值、2.5mM NaOH接受液和30分钟萃取时间。将萃取的药物直接注入CE，在由30mM醋酸铵用醋酸调节至pH 4.2的背景电解质溶液中进行分离和定量。包括药物萃取、进样、分离和定量在内的整个分析过程在CE仪器中实现了自动化，唯一的手动操作是浸渍SLM以及用样品和接受液填充微萃取装置。该分析方法适用于同时测定未稀释人尿样中的碱性和酸性药物，并用于口服Nalgesin S片后尿液中萘普生的直接测定。实现了样品基质的有效消除以及碱性和酸性药物的选择性转移，联用SLM-CE方法的特征在于峰面积的重复性在3.7%至13.4%之间、峰面积与浓度之间呈线性关系（r = 0.994 - 0.999）以及检测限在0.05至1.5μg/mL之间。
