Department of Chemistry and Center for Nanotechnology at CYCU, Chung Yuan Christian University, 200 Chung Pei Road, Chung-Li 320, Taiwan.
J Chromatogr A. 2011 Jan 14;1218(2):350-8. doi: 10.1016/j.chroma.2010.11.040. Epub 2010 Nov 25.
This study describes the ability of on-line concentration capillary electrochromatography (CEC) coupled with UV or mass spectrometry (MS) for the determination of nine common non-steroidal anti-inflammatory drugs (NSAIDs) in water samples. A series of poly(stearyl methacrylate-divinylbenzene) (poly(SMA-DVB)) monolithic columns, which were prepared by single step in situ polymerization of divinylbenzene (DVB), stearyl methacrylate (SMA) and vinylbenzenesulfonic acid (VBSA, charged monomer), were developed as separation columns for the first time. The effects of polymerization condition of monolithic columns on analyte separations were examined, and the results indicated that separation performances were markedly improved in monolithic columns prepared with short reaction time (3 h) and low SMA:DVB ratio (40/60 ratio of SMA:DVB). Subsequently, an on-line concentration step of step-gradient elution was combined to this CEC system, and by optimizing the difference in eluent strength between the sample matrix and mobile phase, all NSAIDs detection sensitivity were improved (limit of detection (LOD) was 3.4-10 μg/L for UV, and 0.01-0.19 μg/L for MS). When compared to the best CE and LC reports on NSAIDs analyses so far, this on-line concentration CEC method provided better detection ability within shorter separation time (12 min) when either UV or MS detector was employed. This is the first report for on-line concentration CEC with MS detection applied in trace solute analyses of real samples.
本研究描述了在线浓缩毛细管电色谱(CEC)与紫外或质谱(MS)联用,用于测定水样中九种常见的非甾体抗炎药(NSAIDs)的能力。首次制备了一系列聚(硬脂基甲基丙烯酸酯-二乙烯基苯)(poly(SMA-DVB))整体柱,该整体柱是通过一步原位聚合二乙烯基苯(DVB)、硬脂基甲基丙烯酸酯(SMA)和乙烯基苯磺酸(VBSA,带电单体)制备而成。考察了聚合条件对整体柱分离性能的影响,结果表明,在聚合时间短(3 h)和 SMA:DVB 比例低(SMA:DVB 为 40/60)的整体柱中,分离性能得到显著提高。随后,将在线浓缩步阶梯度洗脱与该 CEC 系统相结合,并通过优化样品基质与流动相之间的洗脱强度差异,提高了所有 NSAIDs 的检测灵敏度(UV 检测的检出限(LOD)为 3.4-10 μg/L,MS 检测的为 0.01-0.19 μg/L)。与迄今为止 NSAIDs 分析方面的最佳 CE 和 LC 报告相比,当使用 UV 或 MS 检测器时,这种在线浓缩 CEC 方法在更短的分离时间(12 min)内提供了更好的检测能力。这是首次报道将在线浓缩 CEC 与 MS 检测应用于实际样品痕量溶质分析。