Proteo-Science Center, Division of Proteomics Research, Ehime University , Shitsukawa, Toon, Ehime, 791-0295, Japan.
The United Graduate School of Agricultural Sciences, Ehime University , Matsuyama, Ehime, 790-8566, Japan.
Anal Chem. 2017 Aug 15;89(16):8244-8250. doi: 10.1021/acs.analchem.7b00357. Epub 2017 Aug 2.
Biologists' preeminent toolbox for separating, analyzing, and visualizing proteins is SDS-PAGE, yet recovering the proteins embedded in these polyacrylamide media as intact species is a long-standing challenge for mass spectrometry. In conventional workflows, protein mixtures from crude biological samples are electrophoretically separated at high-resolution within N,N'-methylene-bis-acrylamide cross-linked polyacrylamide gels to reduce sample complexity and facilitate sensitive characterization. However, low protein recoveries, especially for high molecular weight proteins, often hinder characterization by mass spectrometry. We describe a workflow for top-down/bottom-up mass spectrometric analyses of proteins in polyacrylamide slab gels using dissolvable, bis-acryloylcystamine-cross-linked polyacrylamide, enabling high-resolution protein separations while recovering intact proteins over a broad size range efficiently. The inferior electrophoretic resolution long associated with reducible gels has been overcome, as demonstrated by SDS-PAGE of crude tissue extracts. This workflow elutes intact proteins efficiently, supporting MS and MS/MS from proteins resolved on biologists' preferred separation platform.
生物学家用于分离、分析和可视化蛋白质的主要工具是 SDS-PAGE,但从这些聚丙烯酰胺介质中回收完整的蛋白质仍然是质谱分析的长期挑战。在传统工作流程中,从粗生物样品中提取的蛋白质混合物在 N,N'-亚甲基双丙烯酰胺交联的聚丙烯酰胺凝胶中进行高分辨率电泳分离,以降低样品复杂性并促进灵敏的特征分析。然而,低蛋白回收率,特别是对于高分子量蛋白质,常常阻碍了通过质谱法进行的特征分析。我们描述了一种使用可溶解的双丙烯酰基半胱胺交联的聚丙烯酰胺在聚丙烯酰胺板凝胶中进行自上而下/自下而上的蛋白质质谱分析的工作流程,该方法能够高效地回收广泛大小范围内的完整蛋白质,同时实现高分辨率的蛋白质分离。我们克服了与还原凝胶相关的较差电泳分辨率的问题,如对粗组织提取物进行 SDS-PAGE 所示。该工作流程可有效地洗脱完整的蛋白质,支持在生物学家首选的分离平台上分离的蛋白质进行 MS 和 MS/MS。