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采用高效薄层色谱-紫外光密度法筛查和测定掺假草药减肥补充剂中的西布曲明。

Screening and determination of sibutramine in adulterated herbal slimming supplements by HPTLC-UV densitometry.

作者信息

Mathon Caroline, Ankli Anita, Reich Eike, Bieri Stefan, Christen Philippe

机构信息

a Official Food and Veterinary Control Authority of Geneva , Quai Ernest-Ansermet 22, CH-1211 Geneva 4 , Switzerland.

出版信息

Food Addit Contam Part A Chem Anal Control Expo Risk Assess. 2014;31(1):15-20. doi: 10.1080/19440049.2013.861934. Epub 2014 Jan 15.

DOI:10.1080/19440049.2013.861934
PMID:24215519
Abstract

The adulteration of herbal supplements is of growing importance, especially when they contain undeclared compounds like sibutramine that are unsafe drugs. Sibutramine was withdrawn from US and European markets in 2010. In this study, an HPTLC-UV densitometric method was developed for the quantification of sibutramine in herbal diet foods. Sample extracts were directly applied onto HPTLC silica gel plates and separated with a mobile phase made of a toluene-methanol mixture. Sibutramine was quantified at 225 nm and its unequivocal identification was confirmed by MS using a TLC-MS interface. During two surveys, 52 weight loss supplements obtained via the Internet were screened. Half of those were adulterated with sibutramine at amounts reaching up to 35 mg per capsule. The results of this validated HPTLC method were compared with those obtained by HPLC-UV and HPLC-MS/MS. The results were not significantly different with the three methods.

摘要

草药补充剂的掺假问题日益重要,尤其是当它们含有西布曲明等未申报的不安全药物成分时。西布曲明于2010年在美国和欧洲市场退市。在本研究中,开发了一种高效薄层色谱-紫外光密度法用于定量草药减肥食品中的西布曲明。将样品提取物直接点样于高效薄层色谱硅胶板上,并用甲苯-甲醇混合流动相进行分离。西布曲明于225nm处进行定量,通过薄层色谱-质谱联用接口的质谱法对其进行明确鉴定。在两项调查中,对通过互联网获得的52种减肥补充剂进行了筛查。其中一半掺有西布曲明,每粒胶囊中西布曲明含量高达35mg。将这种经过验证的高效薄层色谱法的结果与通过高效液相色谱-紫外法和高效液相色谱-串联质谱法获得的结果进行了比较。三种方法的结果没有显著差异。

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