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用于检测N-乙基-α-乙基苯乙胺(ETH)、N,N-二乙基苯乙胺和苯乙胺的膳食补充剂的液相色谱-串联质谱分析。

LC-MS-MS analysis of dietary supplements for N-ethyl-α-ethyl-phenethylamine (ETH), N, N-diethylphenethylamine and phenethylamine.

作者信息

ElSohly Mahmoud A, Gul Waseem

机构信息

1 ElSohly Laboratories, Inc. (ELI) and Phytochemical Services, Incorporated (PSI), 5 Industrial Park Drive, Oxford, MS 38655, USA.

出版信息

J Anal Toxicol. 2014 Mar;38(2):63-72. doi: 10.1093/jat/bkt097. Epub 2013 Dec 15.

Abstract

There has been a recent rise in the number of cases of athletes being banned from competition because of positive tests for prohibited substances in their biological specimens. Most of these substances are on the World Anti-Doping Agency (WADA) prohibited list, while others are not specifically named on the list. N-Ethyl-α-ethyl-phenethylamine (ETH), a derivative of phenethylamine (PEA), is one of these unlisted substances and shares chemical and biological effects to the amphetamines, which are listed on the WADA prohibited substances list. It is classified as Category 6B stimulant on the list. This study was directed toward the development of an liquid chromatography tandem mass spectrometry (LC-MS-MS) method for the analysis of ETH in performance-enhancing dietary supplement. A standard was prepared and confirmed by spectroscopic analysis, which was then used to develop the analytical procedure. The procedure was validated and found to have an limit of detection of 2.5 ng/mL, limit of quantification of 5 ng/mL and upper limit of linearity of 500 ng/mL, with within-day variability at the 10-ng/mL level range of 3.88-7.89% (n = 6) and 1.39-3.36% (n = 6) for the 100-ng/mL level. The day-to-day variability was 9.8% for the low control and 3.1% for the high control. The method was used to analyze a variety of dietary supplements for ETH as well as PEA and its N, N-diethyl derivative (NDP).

摘要

最近,因生物样本中违禁物质检测呈阳性而被禁赛的运动员数量有所增加。这些物质大多在世界反兴奋剂机构(WADA)的禁用清单上,而其他一些则未在清单中具体列出。N-乙基-α-乙基苯乙胺(ETH)是苯乙胺(PEA)的衍生物,是这些未列出的物质之一,其化学和生物学效应与安非他明相似,安非他明被列在WADA禁用物质清单上。它在该清单中被归类为6B类兴奋剂。本研究旨在开发一种液相色谱串联质谱(LC-MS-MS)方法,用于分析增强体能的膳食补充剂中的ETH。制备了一种标准品并通过光谱分析进行了确认,然后用于开发分析程序。该程序经过验证,检测限为2.5 ng/mL,定量限为5 ng/mL,线性上限为500 ng/mL,在10 ng/mL水平的日内变异性为3.88-7.89%(n = 6),在100 ng/mL水平为1.39-3.36%(n = 6)。低浓度对照的日间变异性为9.8%,高浓度对照为3.1%。该方法用于分析各种膳食补充剂中的ETH以及PEA及其N,N-二乙基衍生物(NDP)。

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