US Drug Enforcement Administration, Special Testing and Research Laboratory, 22624 Dulles Summit Court, Dulles, VA 20166, USA.
J Chromatogr A. 2011 Dec 30;1218(52):9336-44. doi: 10.1016/j.chroma.2011.10.067. Epub 2011 Nov 3.
The use of hydrophilic interaction chromatography (HILIC) with sub 2 μm particle columns for the analysis of drugs and related compounds of forensic interest is described. This technique uses a high organic/low aqueous buffered mobile phase with a polar stationary phase, and is excellent for the separation of many of the charged solutes that are found in forensic drug exhibits. In this study, HILIC is investigated for 11 solutes of forensic interest, including weak bases, weak acids, and a neutral solute. In addition, for columns containing either ethylene bridged hybrid particles with or without an amide bonded phase, the effects of acetonitrile concentration, buffer type, buffer concentration, linear velocity, and sample concentration were studied. Based on these studies, HILIC with sub 2 μm particle columns can offer highly efficient, selective, and rapid isocratic separations of drugs and related compounds of forensic interest, with excellent peak shapes and low back pressures. This is in contrast to reverse phase chromatography (RPLC), where gradient elution is usually required, which can result in extensive overlap between acidic, neutral, and basic solutes. In addition, since HILIC exhibits a much greater loading capacity than RPLC, it could be a preferred technique for drug profiling. Furthermore, because high organic content mobile phases are highly amenable to mass spectrometric detection, the use of HILIC with tandem mass spectrometric detection for the analysis of seized drugs is described.
本文描述了亚 2μm 粒径颗粒柱亲水作用色谱(HILIC)在分析法医学感兴趣的药物和相关化合物中的应用。该技术使用高有机/低水缓冲移动相和极性固定相,非常适合分离法医学药物检材中存在的许多带电溶质。在这项研究中,考察了 HILIC 对 11 种法医学感兴趣的溶质的分离效果,包括弱碱、弱酸和中性溶质。此外,还研究了含有或不含有酰胺键合相的乙撑桥联混合颗粒柱,考察了乙腈浓度、缓冲液类型、缓冲液浓度、线性速度和样品浓度的影响。基于这些研究,亚 2μm 粒径颗粒柱的 HILIC 可以提供高效、选择性和快速的等度分离,对法医学感兴趣的药物和相关化合物具有出色的峰形和较低的背压。这与反相色谱(RPLC)形成对比,在 RPLC 中,通常需要梯度洗脱,这会导致酸性、中性和碱性溶质之间广泛重叠。此外,由于 HILIC 的负载能力比 RPLC 大得多,因此它可能是药物分析的首选技术。此外,由于高有机含量的流动相非常适合质谱检测,因此描述了使用 HILIC 与串联质谱检测结合分析缉获药物。