Department of Molecular Biology, The Scripps Research Institute, 10550 North Torrey Pines Road, La Jolla, California 92037, USA.
J Phys Chem B. 2012 Jun 14;116(23):6775-80. doi: 10.1021/jp212401w. Epub 2012 Feb 29.
Aqueous solutions of the detergent Fos-10 (n-decylphosphocholine) without and with addition of the integral membrane protein (IMP) OmpX (outer membrane protein X) have been characterized using pulsed field gradient-stimulated echo (PFG-STE) NMR experiments for measurements of translational diffusion coefficients. Effective diffusion coefficients for Fos-10 micelles in the absence of OmpX were obtained by observation of NMR signals from 10-bromodecan-1-ol that had been inserted into the micelles, and in the presence of OmpX by NMR observation of the protein. It is thus shown that solutions of Fos-10-reconstituted OmpX can be quantitatively described as a mixture of Fos-10 monomers, uniform Fos-10 micelles, and uniform OmpX-containing Fos-10 micelles, with Fos-10 monomers in fast exchange between the pools of these three species. This result establishes an avenue for efficient determination of the effective translational diffusion coefficients of IMP-containing detergent micelles based on observation of the intense detergent NMR signals, which is also applicable with unlabeled IMPs. This monitoring of the species present in a given IMP solution contributes to improved guidelines for rational selection of detergent and buffer conditions in structural studies of integral membrane proteins.
已使用脉冲梯度场激发回波(PFG-STE)NMR 实验对无 integral membrane protein (IMP) OmpX(外膜蛋白 X)和添加 integral membrane protein (IMP) OmpX 的去污剂 Fos-10(正十二烷基磷酸胆碱)水溶液的进行了特性描述,用于测量平动扩散系数。通过观察已插入胶束中的 10-溴代十一烷-1-醇的 NMR 信号,获得了无 OmpX 时 Fos-10 胶束的有效扩散系数,而在有 OmpX 时则通过 NMR 观察蛋白质获得了有效扩散系数。因此,表明 Fos-10 再构成 OmpX 的溶液可以定量描述为 Fos-10 单体、均匀 Fos-10 胶束和均匀 OmpX 含 Fos-10 胶束的混合物,Fos-10 单体在这三种物质的池中快速交换。该结果为基于观察强烈的去污剂 NMR 信号高效确定含 IMP 的去污剂胶束的有效平动扩散系数提供了途径,这也适用于未标记的 IMP。这种对特定 IMP 溶液中存在的物质的监测有助于改进结构研究中合理选择去污剂和缓冲条件的指南 integral membrane protein。