Technical Review

液体クロマトグラフィー核磁気共鳴（LC-NMR）の有効な使い方
—医薬品の類縁物質および代謝物の構造決定を目指して—
How do you use liquid chromatography-nuclear magnetic resonance (LC-NMR) effectively for structural determinations of pharmaceutical impurities and metabolites?

川口謙、中野隆行、木村一雄
Ken Kawaguchi, Takayuki Nakano and Kazuo Kimura

Toray Research Center, Inc., Biological Science Labs. 10-1 Tebiro 6-chome, Kamakura-shi, Kanagawa-ken 248-0036, Japan

Abstract:

Structural determinations of pharmaceutical impurities called as related substances and its metabolites are required in the process of new pharmaceuticals developments. Liquid chromatography-nuclear magnetic resonance (LC-NMR) is a powerful tool for the structural determinations in spite of its low sensitivity. In the case of low molecular weight compounds, amount of target sample needed for LC-NMR measurement using stop-flow method is 1-5 μg per a target peak. The amount is too small for NMR but too large for HPLC. To use LC-NMR effectively for the purpose, some points to keep in mind for selecting mobile phase will be provided besides those for injection of the large amount into column and analysis approach.

Keywords: liquid chromatography-nuclear magnetic resonance (LC-NMR), structural determination, pharmaceutical impurity, related substance, metabolite, high performance liquid chromatography (HPLC)

[Full Text PDF]