Hamilton J A, Era S, Bhamidipati S P, Reed R G
Department of Biophysics, Houseman Medical Research Center, Boston University School of Medicine, MA 02118-2394.
Proc Natl Acad Sci U S A. 1991 Mar 15;88(6):2051-4. doi: 10.1073/pnas.88.6.2051.
Binding of 13C-enriched oleic acid to bovine serum albumin and to three large proteolytic fragments of albumin--two complementary fragments corresponding to the two halves of albumin and one fragment corresponding to the carboxyl-terminal domain--yielded unique patterns of NMR resonances (chemical shifts and relative intensities) that were used to identify the locations of binding of the first 5 mol of oleic acid to the multidomain albumin molecule. The first 3 mol of oleic acid added to intact albumin generated three distinct NMR resonances as a result of simultaneous binding of oleic acid to three heterogeneous sites (primary sites). Two of these resonances were seen upon addition of 1 or 2 mol of oleic acid to fragments representing either the carboxyl-terminal half (residues 307-582) or the carboxyl-terminal domain (residues 377-582); the third resonance was seen upon addition of 1 mol of oleic acid to the fragment representing the amino-terminal half (residues 1-306). The resonance patterns for the fourth and fifth moles of oleic acid added to albumin (secondary sites) could not be duplicated by addition of more oleic acid to individual fragments. These resonance patterns were generated, however, when the two complementary fragments were mixed in equimolar proportions to form an albumin-like complex with a reconstituted middle domain. Thus, two primary fatty acid binding sites are assigned to the carboxyl-terminal domain, one primary site is assigned to the amino-terminal half, and the secondary sites are assigned to the middle domain. This distribution suggests albumin to be a less symmetrical binding molecule than theoretical models predict. This work also demonstrates the power of NMR for the study of microenvironments of individual fatty acid binding sites in specific domains.
富含¹³C的油酸与牛血清白蛋白以及白蛋白的三个大的蛋白水解片段(两个互补片段分别对应白蛋白的两半,一个片段对应羧基末端结构域)的结合产生了独特的核磁共振共振模式(化学位移和相对强度),这些模式被用于确定最初5摩尔油酸与多结构域白蛋白分子的结合位置。添加到完整白蛋白中的最初3摩尔油酸由于油酸同时结合到三个异质位点(主要位点)而产生了三个不同的核磁共振共振。当向代表羧基末端一半(残基307 - 582)或羧基末端结构域(残基377 - 582)的片段中添加1或2摩尔油酸时,可以看到其中两个共振;当向代表氨基末端一半(残基1 - 306)的片段中添加1摩尔油酸时,可以看到第三个共振。添加到白蛋白(次要位点)中的第四和第五摩尔油酸的共振模式不能通过向单个片段中添加更多油酸来复制。然而,当将两个互补片段以等摩尔比例混合以形成具有重组中间结构域的类似白蛋白的复合物时,会产生这些共振模式。因此,两个主要脂肪酸结合位点被指定给羧基末端结构域,一个主要位点被指定给氨基末端一半,次要位点被指定给中间结构域。这种分布表明白蛋白是一个比理论模型预测的对称性更低的结合分子。这项工作还证明了核磁共振在研究特定结构域中单个脂肪酸结合位点的微环境方面的强大作用。