University Children's Hospital, Division of Analytical Biochemistry and Mass Spectrometry, Auenbruggerplatz 34/2, A-8036 Graz, Austria.
Rapid Commun Mass Spectrom. 2010 Nov 30;24(22):3320-4. doi: 10.1002/rcm.4775.
The synthesis of a novel electrophoric derivatisation reagent, o-(pentafluorobenzyloxycarbonyl)benzoyl chloride, is described. The reagent was tested against selected primary and secondary amino compounds as analytical targets. The derivatives exhibit excellent mass spectral properties under negative ion chemical ionisation (NICI), i.e. reduced fragmentation and thus high ion current for the targeted m/z during analysis. Since the reagent bears a pentafluorobenzyl ester group, resulting mass NICI mass spectra were expectedly dominated by dissociative resonance electron capture typically observed with these compounds. The reagent is suitable for detecting volatile primary and secondary amines with high sensitivity. Background is reduced by a shift in detected m/z and retention time, as demonstrated for the analysis of the drug methylphenidate from human plasma.
描述了一种新型的电喷雾衍生试剂 o-(五氟苯甲酰氧基)苯甲酰氯的合成。该试剂被测试用于选择的伯胺和仲胺化合物作为分析目标。在负离子化学电离（NICI）下，这些衍生物表现出优异的质谱性质，即在分析过程中，针对目标 m/z 的碎片减少，因此离子电流高。由于该试剂带有五氟苄酯基团，因此预期所得到的 NICI 质谱主要由与这些化合物通常观察到的解离共振电子俘获主导。该试剂适用于检测具有高灵敏度的挥发性伯胺和仲胺。如对人血浆中甲基苯丙胺的分析所示，通过检测 m/z 和保留时间的变化，可以降低背景。
