Molecular and Cellular Biochemistry Department, Indiana University, Bloomington, Indiana, USA.
Department of Pharmacology, Northwestern University Feinberg School of Medicine, Chicago, Illinois, USA.
Protein Sci. 2024 Jun;33(6):e4976. doi: 10.1002/pro.4976.
G-protein coupled receptors (GPCRs) are the largest class of membrane proteins encoded in the human genome with high pharmaceutical relevance and implications to human health. These receptors share a prevalent architecture of seven transmembrane helices followed by an intracellular, amphipathic helix 8 (H8) and a disordered C-terminal tail (Ctail). Technological advancements have led to over 1000 receptor structures in the last two decades, yet frequently H8 and the Ctail are conformationally heterogeneous or altogether absent. Here we synthesize a peptide comprising the neurotensin receptor 1 (NTS1) H8 and Ctail (H8-Ctail) to investigate its structural stability, conformational dynamics, and orientation in the presence of detergent and phospholipid micelles, which mimic the membrane. Circular dichroism (CD) and nuclear magnetic resonance (NMR) measurements confirm that zwitterionic 1,2-diheptanoyl-sn-glycero-3-phosphocholine is a potent stabilizer of H8 structure, whereas the commonly-used branched detergent lauryl maltose neopentyl glycol (LMNG) is unable to completely stabilize the helix - even at amounts four orders of magnitude greater than its critical micellar concentration. We then used NMR spectroscopy to assign the backbone chemical shifts. A series of temperature and lipid titrations were used to define the H8 boundaries as F376-R392 from chemical shift perturbations, changes in resonance intensity, and chemical-shift-derived phi/psi angles. Finally, the H8 azimuthal and tilt angles, defining the helix orientation relative of the membrane normal were measured using paramagnetic relaxation enhancement NMR. Taken together, our studies reveal the H8-Ctail region is sensitive to membrane physicochemical properties and is capable of more adaptive behavior than previously suggested by static structural techniques.
G 蛋白偶联受体 (GPCRs) 是人类基因组中编码的最大膜蛋白家族,具有很高的药物相关性和对人类健康的影响。这些受体具有共同的七跨膜螺旋结构,其后是细胞内的、两亲性的螺旋 8 (H8) 和无序的 C 末端尾巴 (Ctail)。技术进步使得在过去二十年中获得了超过 1000 个受体结构,但 H8 和 Ctail 经常表现出构象异质性或完全缺失。在这里,我们合成了一个包含神经降压素受体 1 (NTS1) H8 和 Ctail (H8-Ctail) 的肽,以研究其结构稳定性、构象动力学以及在去污剂和磷脂胶束存在下的取向,这些胶束模拟了膜。圆二色性 (CD) 和核磁共振 (NMR) 测量证实,两性离子 1,2-二庚酰基-sn-甘油-3-磷酸胆碱是 H8 结构的有效稳定剂,而常用的支链去污剂月桂基麦芽糖新戊二醇 (LMNG) 则不能完全稳定该螺旋 - 即使在其临界胶束浓度的四个数量级以上的量下也是如此。然后,我们使用 NMR 光谱来分配骨架化学位移。一系列温度和脂质滴定用于根据化学位移扰动、共振强度变化和化学位移衍生的 φ/psi 角度来定义 H8 边界为 F376-R392。最后,使用顺磁弛豫增强 NMR 测量 H8 的方位角和倾斜角,定义相对于膜法线的螺旋取向。总之,我们的研究表明,H8-Ctail 区域对膜的物理化学性质敏感,并且能够表现出比以前基于静态结构技术所认为的更具适应性的行为。