液相色谱-核磁共振联用仪和液相色谱-质谱联用仪对新型抗真菌药物艾考芬净中一种杂质的鉴定
LC-NMR and LC-MS identification of an impurity in a novel antifungal drug icofungipen.
作者信息
Novak Predrag, Tepes Predrag, Ilijas Marina, Fistrić Ines, Bratos Igor, Avdagić Amir, Hamersak Zdenko, Marković Vesna Gabelica, Dumić Miljenko
机构信息
Department of Chemistry, University of Zagreb, Croatia.
出版信息
J Pharm Biomed Anal. 2009 Aug 15;50(1):68-72. doi: 10.1016/j.jpba.2009.03.017. Epub 2009 Mar 25.
Successful use of LC-NMR and LC-MS for rapid identification of an impurity in a novel antifungal drug icofungipen has been demonstrated. Complementary information obtained from the two methods made it possible to determine the structure of A1 prior to its isolation and purification. Stop-flow LC-NMR ((1)H and DQFCOSY), LC-MS and LC-MS/MS spectra have shown that A1 is structurally related to icofungipen. It was later isolated and prepared synthetically and its structure was corroborated by high-resolution NMR spectroscopy.
已证明成功使用液相色谱-核磁共振联用仪（LC-NMR）和液相色谱-质谱联用仪（LC-MS）快速鉴定新型抗真菌药物艾考芬净中的一种杂质。从这两种方法获得的互补信息使得在分离和纯化之前确定A1的结构成为可能。停流LC-NMR（（1）H和DQFCOSY）、LC-MS和LC-MS/MS光谱表明A1在结构上与艾考芬净相关。后来它被分离出来并通过合成制备，其结构通过高分辨率核磁共振光谱得到证实。
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