Department of Organic Chemistry, Pfizer Analytical Research Centre, Ghent University, Krijgslaan 281S4-bis, 9000, Ghent, Belgium.
Anal Bioanal Chem. 2014 Jan;406(2):401-7. doi: 10.1007/s00216-013-7281-7. Epub 2013 Aug 27.
Analysis of drugs and metabolites in biological matrices such as blood or plasma by LC-MS is routinely challenged by the presence of large quantities of competing molecules for ionization in soft ionization sources, such as proteins and phospholipids. While the former can easily be removed by protein precipitation, pre-analytical extraction of the latter is necessary because they show very high retention in reversed-phase LC resulting in long analysis times or in ion suppression effects when not eluted before the next runs. A novel HILIC-based SPE approach, making use of silica cartridges and of acetone as organic solvent, is introduced as a potent alternative to current commercial methods for phospholipid removal. The methodology was developed and tested for a broad polarity range of pharmaceutical solutes (log P from 0 to 6.6) and broad applicability can therefore be envisaged.
采用 LC-MS 分析生物基质（如血液或血浆）中的药物及其代谢物时，通常会受到软电离源中大量竞争分子（如蛋白质和磷脂）电离的影响。虽然可以通过蛋白质沉淀轻松去除前者，但由于后者在反相 LC 中具有非常高的保留性，导致分析时间长或在下一次运行之前未洗脱时会出现离子抑制效应，因此需要对其进行预分析提取。本文介绍了一种基于亲水相互作用色谱（HILIC）的新型 SPE 方法，该方法使用硅胶小柱和丙酮作为有机溶剂，可作为当前商业方法去除磷脂的有效替代方法。该方法是针对广泛极性范围的药物溶质（log P 从 0 到 6.6）进行开发和测试的，因此可以预见其具有广泛的适用性。
