Department of Biochemistry and Molecular Biology, University of Miami Miller School of Medicine, Miami, FL, USA.
Department of Neurology, University of Miami Miller School of Medicine, Miami, FL, USA.
Methods Mol Biol. 2024;2839:249-259. doi: 10.1007/978-1-0716-4043-2_15.
Thiol-disulfide interconversions are pivotal in the intricate chemistry of biological systems. They play a vital role in governing cellular redox potential and shielding against oxidative harm. These interconversions can also act as molecular switches within an expanding array of redox-regulated proteins, facilitating dynamic and responsive processes. Furthermore, metal-binding proteins often use thiols for coordination. Reverse thiol trapping is a valuable analytical tool to study the redox state of cysteines in biological systems. By selectively capturing and stabilizing free thiol species with an alkylating agent, reverse thiol trapping allows for their subsequent identification and quantification. Various methods can be employed to analyze the trapped thiol adducts, including electrophoresis-based methods, mass spectrometry, nuclear magnetic resonance spectroscopy, and chromatographic techniques. In this chapter, we will focus on describing a simple and sensitive method to sequentially block thiols in their cellular state with a cell-permeant agent (iodoacetamide), and following reduction and denaturation of the samples, trap the native disulfides with a second blocker that shifts the apparent molecular weight of the protein. The oxidation status of proteins for which suitable antibodies are available can then be analyzed by immunoblotting. We present examples of mitochondrial proteins that use cysteine thiols to coordinate metal factors such as iron-sulfur clusters, zinc, and copper.
巯基-二硫键转换在生物系统的复杂化学中起着关键作用。它们在调节细胞氧化还原电势和抵御氧化损伤方面起着至关重要的作用。这些转换还可以作为氧化还原调节蛋白中不断扩展的分子开关,促进动态和响应性过程。此外,金属结合蛋白通常使用巯基进行配位。反向巯基捕获是一种研究生物系统中半胱氨酸氧化还原状态的有价值的分析工具。通过使用烷基化剂选择性地捕获和稳定游离巯基物种,可以随后对其进行鉴定和定量。可以采用多种方法分析捕获的巯基加合物,包括电泳方法、质谱、核磁共振波谱和色谱技术。在本章中,我们将重点描述一种简单而灵敏的方法,即用细胞通透性试剂(碘乙酰胺)依次阻断细胞中巯基,然后在还原和变性样品后,用第二个阻断剂捕获天然二硫键,该阻断剂会改变蛋白质的表观分子量。然后可以通过免疫印迹分析具有合适抗体的蛋白质的氧化状态。我们提供了一些使用半胱氨酸巯基来协调铁硫簇、锌和铜等金属因子的线粒体蛋白的例子。