Daeseleire E, De Guesquière A, Van Peteghem C
Laboratory of Food Analysis, Faculty of Pharmaceutical Sciences, State University of Ghent, Belgium.
J Chromatogr. 1991 Apr 5;564(2):445-9. doi: 10.1016/0378-4347(91)80512-b.
A procedure is described for the detection of 17 beta-19-nortestosterone (17 beta-19-NT) and 17 alpha-methyltestosterone (17 alpha-MT) in muscle tissue by a combination of high-performance liquid chromatography and radioimmunoassay. The steroids were released from the muscle tissue by enzyme digestion, and the extracts were purified by solid-phase extraction. A meat sample from the retail trade, which was proved to contain 17 beta-19-NT and 17 alpha-MT residues by gas chromatography-mass spectrometry, and blank meat samples obtained from non-treated experimental animals were purified and the extracts injected into the liquid chromatograph. With an automatic fraction collector, fifteen fractions of 1 ml each were obtained, which after evaporation were subjected to a radioimmunoassay for the steroid concerned. It was demonstrated that none of the fractions from the blank meat samples contains any substance that interfered with the immunochemical detection system. In addition, a good qualitative agreement between the two sets of results was obtained. Although the sample preparation step is rather labour-intensive, the method can be successfully applied as a reliable confirmation method for positive radioimmunoassay screening results in circumstances where no gas chromatography-mass spectrometry facilities are available.
本文描述了一种通过高效液相色谱法和放射免疫分析法相结合来检测肌肉组织中17β-19-去甲睾酮（17β-19-NT）和17α-甲基睾酮（17α-MT）的方法。通过酶消化从肌肉组织中释放出类固醇，提取物通过固相萃取进行纯化。一份来自零售行业的肉类样品，经气相色谱-质谱法证明含有17β-19-NT和17α-MT残留，从未经处理的实验动物获得的空白肉类样品也进行了纯化，并将提取物注入液相色谱仪。使用自动馏分收集器，获得了15个各为1毫升的馏分，蒸发后对相关类固醇进行放射免疫分析。结果表明，空白肉类样品的馏分中均不含有干扰免疫化学检测系统的任何物质。此外，两组结果在定性上具有良好的一致性。尽管样品制备步骤相当耗费人力，但在没有气相色谱-质谱设备的情况下，该方法可成功用作放射免疫分析阳性筛查结果的可靠确证方法。
