Walters M J, Ayers R J, Brown D J
Food and Drug Administration, Detroit, MI 48207.
J Assoc Off Anal Chem. 1990 Nov-Dec;73(6):904-26.
Anabolic steroid products found in the illegal market are primarily oil-based injectables or tablets and often do not contain the ingredients declared on the label. An analytical scheme based on a reverse-phase liquid chromatographic (LC) system for screening, tentative identification, and quantitation is presented. Methanolic sample extracts are chromatographed on an octadecyl column using 2 mobile phases (methanol and (75 + 25) methanol-water) and tracked at 3 wavelengths (240, 210, and 280 nm) or with a photodiode array UV detector. Retention time ratios (RR) relative to testosterone and UV data are used for tentative identification. The same LC system serves as a cleanup and isolation step for identity confirmation by direct insertion probe mass spectrometry (MS) or Fourier transform infrared spectrophotometry (FTIR). Recoveries range from 96.2 to 100.2% for 11 different steroids extracted from sesame oil. LC RR values for over 40 steroids, analytical results for typical products, and MS and FTIR spectra for selected compounds are presented.
在非法市场上发现的合成代谢类固醇产品主要是油基注射剂或片剂,且往往不含有标签上宣称的成分。本文介绍了一种基于反相液相色谱(LC)系统的分析方案,用于筛查、初步鉴定和定量。甲醇样品提取物在十八烷基柱上进行色谱分析,使用两种流动相(甲醇和(75 + 25)甲醇 - 水),并在3个波长(240、210和280 nm)下进行检测,或使用光电二极管阵列紫外检测器。相对于睾酮的保留时间比(RR)和紫外数据用于初步鉴定。相同的LC系统作为净化和分离步骤,通过直接插入探针质谱(MS)或傅里叶变换红外光谱(FTIR)进行身份确认。从芝麻油中提取的11种不同类固醇的回收率在96.2%至100.2%之间。给出了40多种类固醇的LC RR值、典型产品的分析结果以及选定化合物的MS和FTIR光谱。