Di Donna Leonardo, Benabdelkamel Hicham, Taverna Domenico, Indelicato Serena, Aiello Donatella, Napoli Anna, Sindona Giovanni, Mazzotti Fabio
Dipartimento di Chimica e Tecnologie Chimiche, Università della Calabria, Via P. Bucci Cubo 12/C, 87036, Arcavacata di Rende, CS, Italy.
Anal Bioanal Chem. 2015 Jul;407(19):5835-42. doi: 10.1007/s00216-015-8772-5. Epub 2015 May 27.
A method for the determination and quantification of ketosteroid hormones in meat by mass spectrometry, based on the derivatization of the carbonyl moiety of steroids by O-methylhydroxylamine, is presented. The quantitative assay is performed by means of multiple-reaction-monitoring (MRM) scan mode and using the corresponding labelled species, obtained by reaction with d 3-methoxylamine, as internal standard. The accuracy of the method was established by evaluating artificially spiked samples, obtaining values in the range 90-110%. Recovery tests were performed on blank matrix samples spiked with non-natural steroids including trenbolone and melengestrol acetate. The latter experiment revealed that the yield of the extraction processes was approximately 60%. Good values of LOQ and LOD were achieved, making this method competitive with current hormone assay methods.
本文介绍了一种基于用O-甲基羟胺对类固醇羰基部分进行衍生化，通过质谱法测定和定量肉类中酮类固醇激素的方法。定量分析通过多反应监测（MRM）扫描模式进行，并使用与d3-甲氧基胺反应获得的相应标记物作为内标。通过评估人工加标样品确定了该方法的准确性，得到的值在90%-110%范围内。对添加了包括群勃龙和醋酸美仑孕酮在内的非天然类固醇的空白基质样品进行了回收率测试。后一项实验表明，提取过程的产率约为60%。实现了良好的定量限（LOQ）和检测限（LOD）值，使该方法与当前的激素检测方法具有竞争力。
