Jorns M S, Hersh L B
J Biol Chem. 1975 May 25;250(10):3620-8.
N-Methylglutamate synthetase, reconstituted from apo-protein with 5-deazaFMN, catalyzes the reversible formation of N-methylglutamate via the same two-step mechanism previously elucidated for native enzyme (Reactions 1 and 2).(See article). This conclusion is based on the observation that: 1. Enzyme-bound deazaFMN (gamma-max equals 410, 338, epsilon410 equals 10,400 m-minus 1 cm-minus 1) is reduced by L-glutamate, N-methyl-L-glutamate but not D-glutamate. At saturating concentrations of L-glutamate Reaction 1 proceeds at 1% of the rate observed with FMN-reconstituted enzyme. 2. Substrate-reduced deazaFMN enzyme is reoxidized by methylamine or ammonia. 3. A glutaryl enzyme intermediate, isolated by Sephadex G-25 chromatography, contains radioactivity when prepared from [U-14C]glutamate, [alpha-3H]glutamate, or N-[glutaryl U-14C]methylglutamate; however, this intermediate is not labeled from N[methyl 14C]methylglutamate. 4. The amount of radioactivity incorporated into the intermediate is stoichiometric with the amount of deazaFMN reduced during its formation. 5. Intermediate prepared with [U-14C]glutamate yields alpha-[14C]ketoglutarate when denatured with acid and N-[glutaryl-U-14C]methylglutamate when incubated with methylamine. In the absence of methylamine deazaFMN enzyme intermediate slowly decays to yield alpha-hydroxyglutarate. 6. The rate of deazaFMN glutaryl enzyme intermediate formation at a fixed glutamate concentration is equal to the rate of the over-all reaction while the rate of intermediate reaction with methylamine is approximately 50 times greater than the over-all reaction. DeazaFMN enzyme intermediate prepared with [alpha-3H]-glutamate yields [3H]deazaFMNH2 when denatured with acid or phenol and N-[3H]methylglutamate when incubated with methylamine. These results show that the alpha-hydrogen of glutamate is transferred to deazaFMNH2, presumably at the 5 position, during Reaction 1 and that the same hydrogen is utilized for the reformation of the alpha C-H bond during Reaction 2. These results provide the first direct evidence for enzymic hydrogen transfer from substrate to flavin.
用脱氮黄素单核苷酸(5-deazaFMN)从脱辅基蛋白重新组装而成的N-甲基谷氨酸合成酶,通过先前为天然酶阐明的相同两步机制催化N-甲基谷氨酸的可逆形成(反应1和反应2)。(见文章)。这一结论基于以下观察结果:1. 酶结合的脱氮黄素单核苷酸(γ-最大值等于410、338,ε410等于10400 m-1·cm-1)被L-谷氨酸、N-甲基-L-谷氨酸还原,但不被D-谷氨酸还原。在L-谷氨酸饱和浓度下,反应1的进行速度为用黄素单核苷酸(FMN)重新组装的酶所观察到速度的1%。2. 底物还原的脱氮黄素单核苷酸酶被甲胺或氨重新氧化。3. 通过葡聚糖凝胶G-25色谱法分离得到的戊二酰酶中间体,在用[U-14C]谷氨酸、[α-3H]谷氨酸或N-[戊二酰U-14C]甲基谷氨酸制备时含有放射性;然而,该中间体不能被N-[甲基14C]甲基谷氨酸标记。4. 掺入中间体的放射性量与形成过程中还原的脱氮黄素单核苷酸量呈化学计量关系。5. 用[U-14C]谷氨酸制备的中间体在用酸变性时产生α-[14C]酮戊二酸,与甲胺一起孵育时产生N-[戊二酰-U-14C]甲基谷氨酸。在没有甲胺的情况下,脱氮黄素单核苷酸酶中间体缓慢降解产生α-羟基戊二酸。6. 在固定的谷氨酸浓度下,脱氮黄素单核苷酸戊二酰酶中间体的形成速率等于总体反应速率,而中间体与甲胺的反应速率大约比总体反应速率大50倍。用[α-3H]谷氨酸制备的脱氮黄素单核苷酸酶中间体在用酸或苯酚变性时产生[3H]脱氮黄素单核苷酸二氢([3H]deazaFMNH2),与甲胺一起孵育时产生N-[3H]甲基谷氨酸。这些结果表明,在反应1过程中,谷氨酸的α-氢被转移到脱氮黄素单核苷酸二氢上,推测是在5位,并且在反应2过程中,相同的氢被用于重新形成α C-H键。这些结果为酶促氢从底物转移到黄素提供了首个直接证据。