Central Laboratory of the Préfecture de Police of Paris, Paris, France.
Electrophoresis. 2011 Jun;32(11):1282-91. doi: 10.1002/elps.201000626. Epub 2011 Apr 26.
A new CE method was developed for the identification and quantitation of inorganic cations in post-blast residues. The simultaneous analysis in 20 min total runtime of eight cations in post-blast residues (ammonium, potassium, monomethylammonium, calcium, sodium, magnesium, strontium), plus lithium cation as the internal reference, was carried out with a BGE involving a non-CMR (carcinogenic, mutagenic, and harmful to reproduction) chromophore (guanidinium cation) and a double-layer modified capillary (hexadimethrine bromide/polyvinylsulfonate). A study of UV detection conditions using guanidinium ion as the probe led us to set the analysis and reference wavelengths and their associated bandwidths as well as the probe concentration fixed at 15 mM. The successive multiple ionic-polymer layer approach limited the cation adsorption on capillary wall and improved the EOF stability. These caused a significant improvement in method repeatability. Intermediate precisions were 2.4% for corrected areas and 1.3% for normalized migration times. Limits of detection close to 1 mg/L for all cations were obtained. The matrix effects were studied with chemometric approach for different matrices representative of those collected after explosion. Tests with blank matrix extracts of soil, cloth, and with simulated matrix extract containing 800 mg/L Ca²⁺ and 500 mg/L Fe²⁺ were carried out and no significant matrix effects were observed. Finally, analyses of real residues collected after cash dispenser and homemade firework explosions demonstrate excellent correlation between the CE results and those obtained with the ion chromatography method used routinely.
一种新的 CE 方法被开发用于鉴定和定量爆炸残留物中的无机阳离子。在 20 分钟的总运行时间内,同时分析爆炸残留物中的八种阳离子(铵、钾、一甲铵、钙、钠、镁、锶),外加锂离子作为内标,使用包含非 CMR(致癌、致突变和对生殖有害)生色团(胍阳离子)和双层改性毛细管(十六烷基三甲基溴化铵/聚磺酸盐)的 BGE 进行。使用胍离子作为探针对 UV 检测条件的研究使我们能够设置分析和参考波长及其相关带宽,以及将探针浓度固定在 15mM。连续的多离子-聚合物层方法限制了阳离子在毛细管壁上的吸附,并提高了 EOF 的稳定性。这显著提高了方法的重复性。经修正面积的中间精密度为 2.4%,归一化迁移时间的中间精密度为 1.3%。对于所有阳离子,检测限均接近 1mg/L。使用化学计量学方法研究了不同基质的基质效应,这些基质代表了爆炸后收集的那些基质。对土壤、布料的空白基质提取物以及含有 800mg/L Ca²⁺和 500mg/L Fe²⁺的模拟基质提取物进行了测试,未观察到明显的基质效应。最后,对取自自动取款机和自制烟花爆炸后的实际残留物的分析表明,CE 结果与常规使用的离子色谱法获得的结果之间具有极好的相关性。