Desharnais Philippe, Naud Jean-Francois, Ayotte Christiane
INRS-Institut Armand-Frappier, Laboratoire de contrôle du dopage, 531 Boul. des Prairies, Laval, Québec, Canada, H7V 1B7.
Drug Test Anal. 2017 Nov;9(11-12):1744-1752. doi: 10.1002/dta.2320. Epub 2017 Nov 13.
According to the World Anti-Doping Agency (WADA) technical document for erythropoiesis stimulating agents (ESA) analysis (TD2014EPO), double-blotting of serum/plasma samples is mandatory for all analysis by isoelectric focusing (IEF) and for the confirmation procedures (CP) performed by SDS-PAGE or SAR-PAGE. The goal is to prevent potential cross-reactions of the secondary antibody with remaining proteins in the purified samples. To this end, we have developed an immunopurification method of ESA in serum/plasma samples using a combination of streptavidin-coated immunomagnetic beads and biotinylated anti-EPO polyclonal antibodies. Here we report that this immunomagnetic bead-based purification allows the analysis of serum/plasma samples by single-blotting. Serum and plasma samples, either intact or spiked with different ESAs, were immunopurified and analyzed by single-blotting, after SAR-PAGE or IEF using a cross-reaction minimized secondary antibody coupled to HRP. The results show that when samples are immunopurified according to this strategy, there is no non-specific binding when single-blotting is performed after SAR-PAGE. With IEF, we observe a faint smearing, however, in the pH gradient outside the ESA detection region. These interferences did not alter ESA profiles of spiked urinary samples or of samples received for routine testing. This approach was compared to the MAIIA monoliths purification or to the isolation of ESAs with other combinations of immunomagnetic reagents (ie, anti-Mouse IgG-coated magnetic beads and anti-EPO mAb). The recovery of ESAs was shown to be significant for serum/plasma samples. Our results suggest that single-blotting could be performed on serum/plasma samples without non-specific interferences. Copyright © 2017 John Wiley & Sons, Ltd.
根据世界反兴奋剂机构(WADA)关于促红细胞生成素(ESA)分析的技术文件(TD2014EPO),对于所有通过等电聚焦(IEF)进行的分析以及通过SDS-PAGE或SAR-PAGE进行的确认程序(CP),血清/血浆样本的双印迹是必需的。目的是防止二抗与纯化样本中残留蛋白质的潜在交叉反应。为此,我们开发了一种使用链霉亲和素包被的免疫磁珠和生物素化抗EPO多克隆抗体组合在血清/血浆样本中免疫纯化ESA的方法。在此我们报告,这种基于免疫磁珠的纯化允许通过单印迹分析血清/血浆样本。完整的或添加了不同ESA的血清和血浆样本,经免疫纯化后,在使用与HRP偶联的交叉反应最小化二抗进行SAR-PAGE或IEF后,通过单印迹进行分析。结果表明,当按照该策略对样本进行免疫纯化时,在SAR-PAGE后进行单印迹时没有非特异性结合。然而,对于IEF,我们在ESA检测区域之外的pH梯度中观察到微弱的拖尾现象。这些干扰并未改变添加ESA的尿液样本或常规检测样本的ESA图谱。该方法与MAIIA整体柱纯化或与其他免疫磁试剂组合(即抗小鼠IgG包被的磁珠和抗EPO单克隆抗体)分离ESA的方法进行了比较。结果表明,血清/血浆样本中ESA的回收率很高。我们的结果表明,可以对血清/血浆样本进行单印迹且无非特异性干扰。版权所有© 2017 John Wiley & Sons, Ltd.