Rapid screening and structural elucidation of a novel sibutramine analogue in a weight loss supplement: 11-Desisobutyl-11-benzylsibutramine

被引：14

作者：

Mans, Daniel J. ^{[1
]}

Gucinski, Ashley C. ^{[1
]}

Dunn, Jamie D. ^{[1
]}

Gryniewicz-Ruzicka, Connie M. ^{[1
]}

Mecker-Pogue, Laura C. ^{[1
]}

Kao, Jeff L. -F. ^{[2
]}

Ge, Xia ^{[2
]}

机构：

[1] US FDA, CDER Div Pharmaceut Anal, St Louis, MO 63101 USA

[2] Washington Univ, Dept Chem, St Louis, MO 63130 USA

来源：

JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS | 2013年 / 83卷

关键词：

Dietary supplement; Sibutramine; Ion mobility spectrometry; Mass spectrometry; Nuclear magnetic resonance; ION MOBILITY SPECTROMETRY; DIETARY-SUPPLEMENTS; METABOLITES;

D O I：

10.1016/j.jpba.2013.02.031

中图分类号：

O65 [分析化学];

学科分类号：

070302 ; 081704 ;

摘要：

A novel analogue of sibutramine, 11-desisobutyl-11-benzylsibutramine, has been discovered. During routine ion mobility spectrometry (IMS) screening of a weight loss supplement collected at an US FDA import operation facility an unknown peak was observed. Further analysis of the supplement by liquid chromatography-mass spectrometry (LC-MS) and high resolution mass spectrometry revealed an unknown peak with a relative retention time of 1.04 with respect to sibutramine and a predicted formula of C20H24NCl. In order to elucidate the analogue's structure, it was isolated from the supplement and characterized by tandem mass spectrometry and nuclear magnetic resonance (NMR), which revealed the analogue possessed a benzyl moiety at the 11 position in place of the isobutyl group associated with sibutramine. (C) 2013 Published by Elsevier B.V.

引用

页码：122 / 128

页数：7

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