Kimika Fakultatea , Euskal Herriko Unibertsitatea (UPV/EHU) and Donostia International Physics Center (DIPC) , P.K. 1072, 20080 Donostia , Spain.
CIC nanoGUNE , 20018 San Sebastián , Spain.
J Phys Chem B. 2018 Dec 13;122(49):11147-11154. doi: 10.1021/acs.jpcb.8b05975. Epub 2018 Aug 21.
The analysis and interpretation of single molecule force spectroscopy (smFS) experiments is often complicated by hidden effects from the measuring device. Here we investigate these effects in our recent smFS experiments on the ultrafast folding protein gpW, which has been previously shown to fold without crossing a free energy barrier in the absence of force (i.e., downhill folding). Using atomic force microscopy (AFM) smFS experiments, we found that a very small force of ∼5 pN brings gpW near its unfolding midpoint and results in two-state (un)folding patterns that indicate the emergence of a force-induced free energy barrier. The change in the folding regime is concomitant with a 30,000-fold slowdown of the folding and unfolding times, from a few microseconds that it takes gpW to (un)fold at the midpoint temperature to seconds in the AFM. These results are puzzling because the barrier induced by force in the folding free energy landscape of gpW is far too small to account for such a difference in time scales. Here we use recently developed theoretical methods to resolve the origin of the strikingly slow dynamics of gpW under mechanical force. We find that, while the AFM experiments correctly capture the equilibrium distance distribution, the measured dynamics are entirely controlled by the response of the cantilever and polyprotein linker, which is much slower than the protein conformational dynamics. This interpretation is likely applicable to the folding of other small biomolecules in smFS experiments, and becomes particularly important in the case of systems with fast folding dynamics and small free energy barriers, and for instruments with slow response times.
单分子力谱 (smFS) 实验的分析和解释通常受到测量设备隐藏效应的影响。在这里,我们研究了最近在超快折叠蛋白 gpW 的 smFS 实验中的这些效应,此前的研究表明,在没有力的情况下(即顺行折叠),gpW 不会穿过自由能势垒折叠。使用原子力显微镜 (AFM) smFS 实验,我们发现,一个非常小的力约为 5 pN 可以将 gpW 带到其展开中点,并导致二态(展开)折叠模式,表明出现了力诱导的自由能势垒。折叠状态的变化伴随着折叠和解折叠时间的 30,000 倍减慢,从 gpW 在中点温度下(展开)折叠所需的几微秒到 AFM 中的秒。这些结果令人费解,因为力在 gpW 的折叠自由能景观中诱导的势垒太小,无法解释时间尺度的差异。在这里,我们使用最近开发的理论方法来解决 gpW 在机械力下的惊人缓慢动力学的起源。我们发现,虽然 AFM 实验正确地捕获了平衡距离分布,但测量的动力学完全由悬臂和多蛋白接头的响应控制,其速度远慢于蛋白质构象动力学。这种解释可能适用于 smFS 实验中其他小分子的折叠,对于具有快速折叠动力学和小自由能势垒的系统以及具有慢响应时间的仪器,尤其重要。