Department of Physics, Emory University , Atlanta, Georgia 30322, United States.
J Am Chem Soc. 2013 Oct 9;135(40):15077-84. doi: 10.1021/ja404467d. Epub 2013 Oct 1.
Adenosylcobalamin-dependent enzymes accelerate the cleavage of the cobalt-carbon (Co-C) bond of the bound coenzyme by >10(10)-fold. The cleavage-generated 5'-deoxyadenosyl radical initiates the catalytic cycle by abstracting a hydrogen atom from substrate. Kinetic coupling of the Co-C bond cleavage and hydrogen-atom-transfer steps at ambient temperatures has interfered with past experimental attempts to directly address the factors that govern Co-C bond cleavage catalysis. Here, we use time-resolved, full-spectrum electron paramagnetic resonance spectroscopy, with temperature-step reaction initiation, starting from the enzyme-coenzyme-substrate ternary complex and (2)H-labeled substrate, to study radical pair generation in ethanolamine ammonia-lyase from Salmonella typhimurium at 234-248 K in a dimethylsulfoxide/water cryosolvent system. The monoexponential kinetics of formation of the (2)H- and (1)H-substituted substrate radicals are the same, indicating that Co-C bond cleavage rate-limits radical pair formation. Analysis of the kinetics by using a linear, three-state model allows extraction of the microscopic rate constant for Co-C bond cleavage. Eyring analysis reveals that the activation enthalpy for Co-C bond cleavage is 32 ± 1 kcal/mol, which is the same as for the cleavage reaction in solution. The origin of Co-C bond cleavage catalysis in the enzyme is, therefore, the large, favorable activation entropy of 61 ± 6 cal/(mol·K) (relative to 7 ± 1 cal/(mol·K) in solution). This represents a paradigm shift from traditional, enthalpy-based mechanisms that have been proposed for Co-C bond-breaking in B12 enzymes. The catalysis is proposed to arise from an increase in protein configurational entropy along the reaction coordinate.
腺甘钴胺素依赖酶通过 >10(10)倍加速结合辅酶的钴-碳(Co-C)键的断裂。断裂产生的 5'-脱氧腺嘌呤自由基通过从底物中提取氢原子引发催化循环。在环境温度下,Co-C 键断裂和氢原子转移步骤的动力学偶联干扰了过去直接解决控制 Co-C 键断裂催化因素的实验尝试。在这里,我们使用时间分辨、全谱电子顺磁共振波谱,在温度阶跃反应引发下,从酶-辅酶-底物三元复合物和(2)H 标记的底物开始,在二甲基亚砜/水共溶剂系统中,在 234-248 K 下研究来自鼠伤寒沙门氏菌的乙醇胺氨裂解酶中的自由基对生成。(2)H 和(1)H 取代底物自由基形成的单指数动力学相同,表明 Co-C 键断裂速率限制了自由基对的形成。通过使用线性三态模型对动力学进行分析,可以提取 Co-C 键断裂的微观速率常数。Eyring 分析表明,Co-C 键断裂的活化焓为 32 ± 1 kcal/mol,与溶液中的断裂反应相同。因此,酶中 Co-C 键断裂催化的起源是 61 ± 6 cal/(mol·K)(相对于溶液中的 7 ± 1 cal/(mol·K))的大有利活化熵。这代表了从传统的基于焓的机制向 Co-C 键在 B12 酶中断裂的机制的范式转变。该催化被提出是由于反应坐标中蛋白质构象熵的增加。