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使用液相色谱/光电二极管阵列检测器(LC/PDA)和液相色谱/质谱联用仪(LC/MS)测定掺假膳食补充剂中的5型磷酸二酯酶(PDE-5)抑制剂和食欲抑制剂。

Determination of PDE-5 inhibitors and appetite suppressants in adulterated dietary supplements using LC/PDA and LC/MS.

作者信息

Park So-ra, Lee Jin Gyun, Roh Si Hun, Kim Gyudong, Kwon Chan Hyeok, Park Hee Ra, Kwon Ki Sung, Kim Deukjoon, Kwon Sung Won

机构信息

a College of Pharmacy and Research Institute of Pharmaceutical Sciences, Seoul National University , Seoul , Republic of Korea.

出版信息

Food Addit Contam Part B Surveill. 2012;5(1):29-32. doi: 10.1080/19393210.2012.656706. Epub 2012 Mar 1.

Abstract

There have been a number of reports of dietary supplements contaminated with illegal adulterants that threaten consumers' health because of their adverse pharmacological effects. In the present study, a convenient and economic method was developed to detect illegal pharmaceutics, such as PDE-5 inhibitor and appetite suppressants, using liquid chromatography (LC)/photodiode array (PDA) for screening and LC/mass spectrometry (MS) for successive confirmation. Target peaks were identified by comparison of their chromatographic retention times and PDA spectra with those of synthetic standards and finally confirmed by LC/MS. As a result, tadalafil, a PDE-5 inhibitor, and N-desmethylsibutramine, a derivative of sibutramine, were detected in various dietary supplements at concentrations of 13.5-21.9 mg and 3.0 mg per single dose, respectively. The present study will contribute to the development of an analytical method enabling rapid screening of a variety of health foods, and the result suggests that consumers should be aware of serious health risks related to these illegal compounds.

摘要

已有多项关于膳食补充剂被非法掺假物污染的报道,这些掺假物因其不良药理作用而威胁消费者健康。在本研究中,开发了一种简便且经济的方法来检测非法药物,如磷酸二酯酶-5(PDE-5)抑制剂和食欲抑制剂,使用液相色谱(LC)/光电二极管阵列(PDA)进行筛选,并使用LC/质谱(MS)进行后续确认。通过将目标峰的色谱保留时间和PDA光谱与合成标准品的进行比较来鉴定目标峰,最后通过LC/MS进行确认。结果,在各种膳食补充剂中分别检测到浓度为每单剂量13.5 - 21.9毫克的PDE-5抑制剂他达拉非和西布曲明衍生物N-去甲基西布曲明,浓度为每单剂量3.0毫克。本研究将有助于开发一种能够快速筛选各种健康食品的分析方法,结果表明消费者应意识到与这些非法化合物相关的严重健康风险。

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