Grosse Sylvia, Letzel Thomas
Analytical Research Group, Chair of Biopolymer Chemistry, Department of Basic Life Sciences, Technical University of Munich, Freising--Weihenstephan, Germany.
J Chromatogr A. 2007 Jan 12;1139(1):75-83. doi: 10.1016/j.chroma.2006.10.086. Epub 2006 Nov 27.
The analytical hyphenation of micro-flow high-performance liquid chromatography (LC), with post-column liquid mixing and mass spectrometric detection (MS) was established to detect partially oxidized polycyclic aromatic hydrocarbons (oxy-PAHs) for low quantity samples. 100pmol injections of 30 reference standards could be detected in good sensitivity using either atmospheric pressure chemical ionization (APCI) and/or atmospheric pressure photoionization (APPI). The connected mass spectrometer was a single quadrupol analyzer realizing simultaneous registration of positive and negative ions in scan range width of 200 - 300Da. The ionization efficiency was compared using three ionization sources (incl. electrospray ionization (ESI)) for several oxy-PAHs. According to the mass spectra, the analytes behave differently in ionization properties. Ionization mechanism (e.g. deprotonated ions and electron captured ions) could be discussed with new inside views. Finally, the hyphenated system was applied to an exemplary aerosol extract and thus highlighting the expedient utilization of this downscaled method for real samples.
建立了微流高效液相色谱(LC)与柱后液体混合及质谱检测(MS)的联用分析方法,用于检测低含量样品中的部分氧化多环芳烃(oxy-PAHs)。使用大气压化学电离(APCI)和/或大气压光电离(APPI),可以以良好的灵敏度检测100皮摩尔进样量的30种参考标准物。所连接的质谱仪为单四极杆分析仪,可在200 - 300Da的扫描范围宽度内同时记录正离子和负离子。使用三种电离源(包括电喷雾电离(ESI))对几种oxy-PAHs的电离效率进行了比较。根据质谱图,分析物在电离特性上表现不同。可以从新的视角讨论电离机制(如去质子化离子和电子捕获离子)。最后,将该联用系统应用于一个示例性气溶胶提取物,从而突出了这种缩微方法对实际样品的便捷应用。