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在液相色谱/电喷雾电离串联质谱法(LC/ESI-MS/MS)中用作衍生化试剂的含硫脲部分的化合物:羧酸衍生化试剂的合成

Compounds having thiourea moiety as derivatization reagents in liquid chromatography/electrospray ionization-tandem mass spectrometry (LC/ESI-MS/MS): synthesis of derivatization reagents for carboxylic acids.

作者信息

Inoda Hirotaka, Nishiyama Taihei, Yoshikado Takashi, Suwanai Yusuke, Santa Tomofumi

机构信息

Graduate School of Pharmaceutical Sciences, The University of Tokyo, Hongo, Bunkyo-ku, Japan.

出版信息

Biomed Chromatogr. 2011 Jun;25(6):635-40. doi: 10.1002/bmc.1501. Epub 2010 Sep 1.

Abstract

The derivatization reagents for carboxylic acids, N-(Pyridin-3-yl)hydrazinecarbothioamide, N-[4-(dimethylamino)phenyl]hydrazinecarbothioamide, 1-(2-aminoethyl)-3-(pyridin-3-yl)thiourea, 1-(2-aminoethyl)-3-[4-(dimethylamino)phenyl]thiourea and 4-(2-aminoethyl)-N-phenylpiperazine-1-carbothioamide were synthesized. These reagents reacted with carboxylic acids at 60°C for 45 min in the presence of the condensation reagents. The generated derivatives were favorably separated on the reversed-phase column and sensitively detected by electrospray ionization tandem mass spectrometry. These reagents enhanced the electrospray ionization response of the analyte and generated a particular product ion efficiently by collision-induced dissociation, and thus they were suitable for MS/MS detection.

摘要

合成了用于羧酸的衍生化试剂,即N-(吡啶-3-基)肼基硫代甲酰胺、N-[4-(二甲基氨基)苯基]肼基硫代甲酰胺、1-(2-氨基乙基)-3-(吡啶-3-基)硫脲、1-(2-氨基乙基)-3-[4-(二甲基氨基)苯基]硫脲和4-(2-氨基乙基)-N-苯基哌嗪-1-碳硫酰胺。这些试剂在缩合试剂存在下于60°C与羧酸反应45分钟。生成的衍生物在反相柱上得到良好分离,并通过电喷雾电离串联质谱进行灵敏检测。这些试剂增强了分析物的电喷雾电离响应,并通过碰撞诱导解离有效地产生特定的产物离子,因此它们适用于串联质谱检测。

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