Igoli John O, Blackburn Gavin, Gray Alexander I, Sutcliffe Oliver B, Watson David G, Euerby Melvin R, Skellern Graham G
Pharmaceutical Sciences Group, Strathclyde Institute of Pharmacy and Biomedical Sciences, University of Strathclyde, The John Arbuthnott Building, 161 Cathedral Street, Glasgow, G4 0RE, Scotland.
Anal Bioanal Chem. 2015 Feb;407(4):1171-80. doi: 10.1007/s00216-014-8337-z. Epub 2014 Dec 17.
The chromatographic isolation and characterisation of the four compounds present in the quaternary phenanthridine veterinary trypanocidal agent, isometamidium chloride hydrochloride (ISM), is reported. The isolated compounds were unambiguously characterised using spectroscopic (NMR, UV, IR and MS) methods as 3-amino-8-[3-(3-carbamimidoyl-phenyl)-triazenyl]-5-ethyl-6-phenylethidium (1a) and related isomers, 8-amino-3-[3-(3-carbamimidoyl-phenyl)-triazenyl]-5-ethyl-6-phenylethidium, 3,-8-diamino-7-[3-(3-carbamimidoyl-phenyl)-triazenyl]-5-ethyl-6-phenylethidium and 3,-8-bis[3-(3-carbamimidoyl-phenyl)-triazenyl]-5-ethyl-6-phenylethidium. During the course of this study, it was realised that the nature of the solvent used in the NMR study was critical as in DMSO-d6 the quaternary group in the compounds was reduced to dihydro forms (e.g. 2a).
报道了对季铵型菲啶类兽用杀锥虫剂盐酸异美铵（ISM）中存在的四种化合物进行色谱分离和表征的过程。使用光谱法（核磁共振、紫外、红外和质谱）明确鉴定出分离出的化合物为3-氨基-8-[3-(3-氨基甲酰亚氨基苯基)-三氮烯基]-5-乙基-6-苯基乙锭（1a）及其相关异构体，8-氨基-3-[3-(3-氨基甲酰亚氨基苯基)-三氮烯基]-5-乙基-6-苯基乙锭、3,8-二氨基-7-[3-(3-氨基甲酰亚氨基苯基)-三氮烯基]-5-乙基-6-苯基乙锭和3,8-双[3-(3-氨基甲酰亚氨基苯基)-三氮烯基]-5-乙基-6-苯基乙锭。在本研究过程中，人们意识到核磁共振研究中所用溶剂的性质至关重要，因为在氘代二甲亚砜中，化合物中的季铵基团会还原为二氢形式（如2a）。
