Macià Alba, Borrull Francesc, Calull Marta, Aguilar Carme
Departament de QuímicaAnalítica i Química Orgànica, Universitat Rovira i Virgili, Tarragona, Spain.
Electrophoresis. 2005 Feb;26(4-5):970-979. doi: 10.1002/elps.200410239.
Various strategies have been investigated for separating a group of nonsteroidal anti-inflammatory drugs (NSAIDs) by microemulsion electrokinetic capillary chromatography (MEEKC) using high-speed separations. The parameters that of affect the separation, such as the nature of the oil droplet and the buffer, and the surfactant concentration have been studied. In addition, several organic solvents were used to decrease the retention of the analytes in the oil droplet phase and to improve the resolution of the NSAIDs. The optimum microemulsion background electrolyte (BGE) solution made of 0.8% w/w ethyl acetate, 6.6% w/w butan-1-ol, 6.0% w/w acetonitrile, 1.0% w/w sodium dodecyl sulfate (SDS), and 85.6% w/w of 10 mM sodium tetraborate at pH 9.2 resolved the drugs within 8 min. The short-end injection procedure is an alternative for reducing the analysis time. When this procedure was used, the microemulsion BGE solution consisted of 0.8% w/w ethyl acetate, 6.6% w/w butan-1-ol, 17.0% w/w methanol, 1.0% w/w SDS, and 74.6% w/w of 10 mM sodium tetraborate, pH 9.2, and the NSAIDs were separated within 3 min. The reversed electrode polarity stacking mode (REPSM) technique was applied to the on-line concentration of the NSAIDs. In this technique, the sample matrix was pumped out of the capillary using a polarity-switching step. When this technique was applied, the sensitivity was enhanced up to 40-fold and the limits of detection (LODs) were in the low microg.L(-1) levels.
人们已经研究了多种策略,通过微乳液电动毛细管色谱法(MEEKC)并采用高速分离来分离一组非甾体抗炎药(NSAIDs)。研究了影响分离的参数,如油滴和缓冲液的性质以及表面活性剂浓度。此外,还使用了几种有机溶剂来减少分析物在油滴相中的保留,并提高NSAIDs的分离度。由0.8%(w/w)乙酸乙酯、6.6%(w/w)丁醇、6.0%(w/w)乙腈、1.0%(w/w)十二烷基硫酸钠(SDS)和85.6%(w/w)的10 mM硼酸钠(pH 9.2)组成的最佳微乳液背景电解质(BGE)溶液可在8分钟内分离出这些药物。短端进样程序是减少分析时间的一种替代方法。使用该程序时,微乳液BGE溶液由0.8%(w/w)乙酸乙酯、6.6%(w/w)丁醇、17.0%(w/w)甲醇、1.0%(w/w)SDS和74.6%(w/w)的10 mM硼酸钠(pH 9.2)组成,NSAIDs在3分钟内即可分离。反向电极极性堆积模式(REPSM)技术被应用于NSAIDs的在线富集。在该技术中,通过极性切换步骤将样品基质从毛细管中泵出。应用该技术时,灵敏度提高了40倍,检测限(LODs)处于低微克·升⁻¹水平。