Departament de Química Analítica i Química Orgànica, Facultat de Química, Universitat Rovira i Virgili, Marcel·lí Domingo s/n, 43007 Tarragona, Spain.
Anal Bioanal Chem. 2011 Apr;400(2):527-34. doi: 10.1007/s00216-011-4758-0. Epub 2011 Feb 23.
A rapid method for the simultaneous determination of several non-steroidal anti-inflammatory drugs (NSAIDs) in human plasma and urine was developed using transient pseudo-isotachophoresis (ITP) in capillary zone electrophoresis (CZE). The influence of different parameters on resolution and preconcentration efficiency, such as background electrolyte (BGE) composition, sample injection, sample matrix composition, and pH, were studied to optimize the transient pseudo-ITP performance. Optimized conditions were a BGE consisting of 100 mM Na(2)B(4)O(7) in 10% aqueous MeOH solution and hydrodynamic injection of the sample at 50 mbar for 90 s. The sample was prepared in a solution mixture of 1% NaCl/ethanol (30:70 v/v) at pH 10. Our results show that this simple strategy offers improved sensitivity compared to conventional CZE analysis, reaching a 45-fold preconcentration factor. The detection limits (LODs) were as low as 0.07 mg/L for standard samples with good repeatability (values of relative standard deviation, %RSD < 11%). The method was applied to the analysis of NSAIDs in biological samples. Validation for human plasma and urine samples demonstrated good linearity, low detection limits, and satisfactory repeatability values.
建立了一种在毛细管区带电泳（CZE）中采用瞬态拟电泳（ITP）同时测定人血浆和尿液中几种非甾体抗炎药（NSAIDs）的快速方法。研究了不同参数对分辨率和预浓缩效率的影响，如背景电解质（BGE）组成、样品进样、样品基质组成和 pH 值，以优化瞬态拟 ITP 性能。优化条件为 BGE 由 100 mM Na2B4O7 在 10%水甲醇溶液组成，以 50 mbar 的压力进行 90 s 的样品液压进样。样品在 pH 10 的 1%NaCl/乙醇（30:70 v/v）溶液混合物中制备。结果表明，与传统 CZE 分析相比，这种简单的策略可提高灵敏度，达到 45 倍的预浓缩因子。标准样品的检测限（LOD）低至 0.07 mg/L，重复性良好（相对标准偏差值，%RSD < 11%）。该方法应用于生物样品中 NSAIDs 的分析。对人血浆和尿液样品的验证表明，该方法具有良好的线性、低检测限和令人满意的重复性值。
