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在膳食补充剂中鉴定出设计类固醇雄甾烷-3,5-二烯-7,17-二酮。

Identification of the designer steroid Androsta-3,5-diene-7,17-dione in a dietary supplement.

机构信息

U.S. Food and Drug Administration, Forensic Chemistry Center, Cincinnati, OH, United States.

出版信息

Drug Test Anal. 2019 Jul;11(7):1109-1115. doi: 10.1002/dta.2589. Epub 2019 May 3.

Abstract

A liquid chromatography-mass spectrometry (LC-MS) screen for known anabolic-androgenic steroids in a dietary supplement product marketed for "performance enhancement" detected an unknown compound having steroid-like spectral characteristics. The compound was isolated using high performance liquid chromatography with ultraviolet detection (HPLC-UV) coupled with an analytical scale fraction collector. After the compound was isolated, it was then characterized using gas chromatography with simultaneous Fourier Transform infrared detection and mass spectrometry (GC-FT-IR-MS), liquid chromatography-high resolution accurate mass-mass spectrometry (LC-HRAM-MS) and nuclear magnetic resonance (NMR). The steroid had an accurate mass of m/z 285.1847 (error-0.57 ppm) for the protonated species [M + H] , corresponding to a molecular formula of C H O . Based on the GC-FT-IR-MS data, NMR data, and accurate mass, the compound was identified as androsta-3,5-diene-7,17-dione. Although this is not the first reported identification of this designer steroid in a dietary supplement, the data provided adds information for identification of this compound not previously reported. This compound was subsequently detected in another dietary supplement product, which contained three additional active ingredients.

摘要

一种用于“性能提升”的膳食补充剂产品的已知合成代谢雄性类固醇的液相色谱-质谱(LC-MS)筛选检测到一种具有类固醇样光谱特征的未知化合物。使用高效液相色谱法与紫外检测(HPLC-UV)结合分析规模的馏分收集器对该化合物进行了分离。在化合物分离后,使用气相色谱法与同时傅里叶变换红外检测和质谱(GC-FT-IR-MS)、液相色谱-高分辨率精确质量-质谱(LC-HRAM-MS)和核磁共振(NMR)对其进行了表征。该类固醇的质子化物种 [M+H]+ 的精确质量为 m/z 285.1847(误差-0.57 ppm),对应的分子式为 C H O 。基于 GC-FT-IR-MS 数据、NMR 数据和精确质量,该化合物被鉴定为雄甾-3,5-二烯-7,17-二酮。虽然这不是膳食补充剂中首次报道的这种设计类固醇的鉴定,但提供的数据增加了之前未报道的这种化合物的鉴定信息。该化合物随后在另一种膳食补充剂产品中被检测到,其中还含有另外三种活性成分。

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