Blasco Cristina, Van Poucke Christof, Van Peteghem Carlos
Laboratori de Bromatologia i Toxicologia, Facultat de Farmàcia, Universitat de Valencia, Av. Vicent Andrés Estellés s/n, 46100 Burjassot, València, Spain.
J Chromatogr A. 2007 Jun 22;1154(1-2):230-9. doi: 10.1016/j.chroma.2007.03.090. Epub 2007 Mar 30.
A rapid, specific and highly sensitive multi-residue method for the determination of anabolic steroid residues in bovine, pork and poultry muscle tissues was developed. The sample preparation involves enzymatic digestion followed by extraction with methanol. The crude extract was cleaned up by solid-phase extraction (SPE) combining C18 and NH2 columns. The detection was carried out by a highly sensitive liquid chromatography/electrospray ionization tandem mass spectrometry (LC/ESI-MS/MS) method using both positive and negative ionization modes. Natural and synthetic steroids covering different polarities could be extracted, concentrated and purified using one single method. Mobile phase composition and additives were optimized to achieve the highest sensitivity. The linearity was not good enough for quantitative analysis but the method was well-suited for qualitative confirmation. The method was validated according to the European Commission Decision 2002/657/EC. Decision limits (CCalpha) and detection capabilities (CCbeta) were below 0.5 ng g(-1) for all the compounds in the three types of meat studied. The developed method is suitable for routine analysis in our laboratories.
建立了一种快速、特异且高度灵敏的多残留方法，用于测定牛、猪和家禽肌肉组织中的合成代谢类固醇残留。样品制备包括酶解，然后用甲醇萃取。粗提物通过结合C18和NH2柱的固相萃取（SPE）进行净化。采用高灵敏度液相色谱/电喷雾电离串联质谱（LC/ESI-MS/MS）法，在正、负离子模式下进行检测。使用单一方法即可提取、浓缩和纯化涵盖不同极性的天然和合成类固醇。对流动相组成和添加剂进行了优化，以实现最高灵敏度。该方法的线性对于定量分析而言不够理想，但非常适合定性确证。该方法根据欧盟委员会第2002/657/EC号决定进行了验证。在所研究的三种肉类中，所有化合物的决策限（CCalpha）和检测能力（CCbeta）均低于0.5 ng g(-1)。所建立的方法适用于我们实验室的常规分析。
