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采用液相色谱-四极杆线性离子阱质谱法分析健康补充剂中掺假的40种减肥化合物。

Analysis of 40 weight loss compounds adulterated in health supplements by liquid chromatography quadrupole linear ion trap mass spectrometry.

作者信息

Zeng Yun, Xu Yimin, Kee Chee-Leong, Low Min-Yong, Ge Xiaowei

机构信息

Pharmaceutical Laboratory, Applied Sciences Group, Health Sciences Authority, 11 Outram Road, Singapore, 169078, Malaysia.

出版信息

Drug Test Anal. 2016 Mar-Apr;8(3-4):351-6. doi: 10.1002/dta.1846. Epub 2015 Aug 25.

Abstract

In this study, a liquid chromatography-tandem mass spectrometry (LC-MS/MS) with scheduled multiple reaction monitoring (MRM) enhanced product ion (EPI) method was developed for simultaneous determination of 40 compounds with weight loss effect, including bisacodyl, phenolphthalein, and sibutramine and its metabolites, etc. They might be adulterated in health supplements to get prominent weight loss effect. The samples were analyzed using a Q-Trap 5500 coupled with high performance liquid chromatography (HPLC) and a CORTECS ultra performance liquid chromatography (UPLC) C18 column (100 mm x 2.1 mm x1.6 µm). Scheduled MRM was used as survey scan, MS2 spectra acquired in the EPI mode were used to perform library searching to increase the confidence of detection. Limits of detection were less than 10 ng/g for the majority of the analytes. A total of 447 weight loss products were tested in our laboratory in the past three years. Among these samples, 119 samples were found to be adulterated with one or more weight loss compounds, including sibutramine, its metabolites benzyl sibutramine and desmethyl sibutramine; phenolphthalein; bisacodyl; furosemide; liothyronine (T3); and thyroxine (T4). Copyright © 2015 John Wiley & Sons, Ltd.

摘要

在本研究中,开发了一种采用定时多反应监测(MRM)增强产物离子(EPI)模式的液相色谱-串联质谱法(LC-MS/MS),用于同时测定40种具有减肥功效的化合物,包括比沙可啶、酚酞、西布曲明及其代谢物等。这些化合物可能被掺入健康补充剂中以获得显著的减肥效果。样品采用配备高效液相色谱(HPLC)的Q-Trap 5500和CORTECS超高效液相色谱(UPLC)C18柱(100 mm×2.1 mm×1.6 µm)进行分析。定时MRM用作全扫描,在EPI模式下采集的MS2谱图用于进行谱库检索以提高检测的可信度。大多数分析物的检测限低于10 ng/g。在过去三年中,我们实验室共检测了447种减肥产品。在这些样品中,发现有119个样品掺有一种或多种减肥化合物,包括西布曲明及其代谢物苄基西布曲明和去甲基西布曲明;酚酞;比沙可啶;呋塞米;三碘甲状腺原氨酸(T3);以及甲状腺素(T4)。版权所有© 2015约翰威立父子有限公司。

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