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In-line coupling of supported liquid membrane extraction to capillary electrophoresis for simultaneous analysis of basic and acidic drugs in urine
Journal of Chromatography A ( IF 4.1 ) Pub Date : 2017-09-07 , DOI: 10.1016/j.chroma.2017.08.084
Pavla Pantůčková , Pavel Kubáň

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 20 μL of sample and 10 μL of acceptor solution, which were interspaced by the SLM impregnated with 5 μL 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, 2.5 mM NaOH acceptor solution and 30 min extraction time. The extracted drugs were directly injected into CE for separation and quantification in a background electrolyte solution consisting of 30 mM 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 (r2 = 0.994–0.999) and limits of detection between 0.05 and 1.5 μg/mL.



中文翻译:

支持液膜萃取与毛细管电泳的在线耦合,可同时分析尿液中的碱性药物和酸性药物

演示了同时通过薄支撑液膜(SLM)提取碱性药物和酸性药物,以及将提取的药物从SLM表面直接注入毛细管电泳(CE)的方法。与商用CE仪器的进样系统兼容的微萃取设备中,装有20μL样品和10μL受主溶液,这些溶液由浸渍有5μL有机溶剂的SLM隔开。在优化的条件下获得了三种碱性药物(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,包括1-乙基-2-硝基苯作为SLM溶剂,样品溶液的天然pH,2.5 mM NaOH受体溶液和30分钟的提取时间。将提取的药物直接注入CE中,以在背景电解质溶液中进行分离和定量,该背景电解质溶液由30 mM乙酸铵(已用乙酸调节至pH 4.2)组成。整个分析过程(包括药物提取,注射,分离和定量)在CE仪器中都是自动化的,唯一的手动过程是SLM浸渍,并在微萃取装置中充满样品和受体溶液。该分析方法适用于同时测定未稀释的人类尿液样品中的碱性药物和酸性药物,并用于口服纳尔金素S片剂后直接测定尿液中萘普生的含量。2  = 0.994–0.999),检出限在0.05和1.5μg/ mL之间。

更新日期:2017-09-07
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