Alexandrescu Lauren, Lessin William, Lander Gabriel C
Department of Integrative Structural and Computational Biology, Scripps Research; La Jolla, CA 92037, USA.
Skaggs Graduate School of Chemical and Biological Sciences, Scripps Research; La Jolla, CA 92037, USA.
bioRxiv. 2025 Jul 26:2025.07.22.666177. doi: 10.1101/2025.07.22.666177.
Biological reactions often involve macromolecules that undergo substrate-induced conformational changes in under a second, yet capturing these transient states remains challenging. While high-resolution structural techniques such as X-ray crystallography and cryo-electron microscopy (cryo-EM) have advanced our mechanistic understanding of protein-substrate interactions, traditional sample preparation methods are too slow to capture rapid biochemical events. Time-resolved cryo-EM has emerged as a promising approach to visualize structural dynamics on microsecond-to-millisecond timescales, but its widespread adoption has been limited by costly equipment and challenges in achieving rapid mixing, application, and vitrification of samples in a reproducible manner. To address these limitations, we developed "Mix-it-up" (MIU), a modified spray device designed for rapid on-grid mixing and vitrification of cryo-EM samples. By manually applying one sample onto the EM grid, blotting, and subsequently spraying the second sample, we achieve on-grid mixing with a vitrification delay of as low as ~120 milliseconds. We demonstrate MIU's time-resolved capabilities through high-resolution structure determination of mixed samples, pH-induced viral capsid contraction, and ligand-dependent complex formation. These findings establish MIU as a cost-effective, versatile tool for studying rapid biochemical processes and lay the groundwork for future applications to time-resolved cryo-EM.
生物反应通常涉及大分子,这些大分子会在不到一秒的时间内发生底物诱导的构象变化,然而捕获这些瞬态仍然具有挑战性。虽然诸如X射线晶体学和冷冻电子显微镜(cryo-EM)等高分辨率结构技术增进了我们对蛋白质-底物相互作用机制的理解,但传统的样品制备方法太慢,无法捕获快速的生化事件。时间分辨冷冻电子显微镜已成为一种有前景的方法,可在微秒到毫秒的时间尺度上可视化结构动力学,但其广泛应用受到昂贵设备以及以可重复方式实现样品快速混合、施加和玻璃化方面挑战的限制。为了解决这些限制,我们开发了“Mix-it-up”(MIU),这是一种经过改进的喷雾装置,专为冷冻电子显微镜样品的快速在网格上混合和玻璃化而设计。通过手动将一种样品施加到电子显微镜网格上,吸干,然后喷洒第二种样品,我们实现了在网格上的混合,玻璃化延迟低至约120毫秒。我们通过对混合样品进行高分辨率结构测定、pH诱导的病毒衣壳收缩以及配体依赖性复合物形成来证明MIU的时间分辨能力。这些发现确立了MIU作为研究快速生化过程的一种经济高效、多功能的工具,并为未来在时间分辨冷冻电子显微镜中的应用奠定了基础。