Daubner S C, Matthews R G
J Biol Chem. 1982 Jan 10;257(1):140-5.
Methylenetetrahydrofolate reductase from pig liver has been purified to homogeneity, as judged by several criteria: (i) a single band with a subunit molecular weight of 77,300 following polyacrylamide gel electrophoresis in the presence of sodium dodecyl sulfate; (ii) a molecular weight determined by amino acid analysis of 74,500 per flavin, in agreement with the subunit molecular weight; and (iii) constant specific activities in the peak fractions during the final chromatography step. The purified enzyme exhibits a typical flavoprotein absorption spectrum. Methylenetetrahydrofolate reductase is a minor constituent of pig liver, and to obtain homogeneous enzyme, a 32,000-fold purification must be accomplished. The preparation described herein attains such purification in 5 steps and with a 14% yield. The enzyme isolated in this fashion is active and stable, and contains a stoichiometric complement of FAD. The enzyme is reducible under anaerobic conditions by 5-deazaflavin/EDTA/light or by NADPH. Reduction of 1 mol of enzyme-bound FAD requires 1.1 mol of NADPH. The reduced enzyme can be reoxidized by (6-R)-methylenetetrahydrofolate, again with nearly 1:1 stoichiometry. Steady state kinetic measurements of the NADPH-methylenetetrahydrofolate oxidoreductase activity give parallel line double reciprocal plots. The turnover number per mol of enzyme-bound flavin is 1600/min under Vmax conditions. The spectrum of the enzyme-bound flavin is significantly perturbed by the binding of S-adenosylmethionine, a metabolite known to be an allosteric modulator of the enzyme.
通过以下几个标准判断,猪肝中的亚甲基四氢叶酸还原酶已被纯化至同质:(i)在十二烷基硫酸钠存在下进行聚丙烯酰胺凝胶电泳后,出现一条亚基分子量为77,300的单一谱带;(ii)通过氨基酸分析确定的每黄素分子量为74,500,与亚基分子量一致;(iii)在最终色谱步骤中,峰级分中的比活性恒定。纯化后的酶呈现出典型的黄素蛋白吸收光谱。亚甲基四氢叶酸还原酶是猪肝中的一种次要成分,为获得同质酶,必须完成32,000倍的纯化。本文所述的制备方法通过5个步骤实现了这种纯化,产率为14%。以这种方式分离的酶具有活性且稳定,并含有化学计量的FAD。该酶在厌氧条件下可被5-脱氮黄素/EDTA/光或NADPH还原。还原1摩尔与酶结合的FAD需要1.1摩尔NADPH。还原后的酶可被(6-R)-亚甲基四氢叶酸再次氧化至近1:1的化学计量比。对NADPH-亚甲基四氢叶酸氧化还原酶活性进行稳态动力学测量,得到平行线双倒数图。在Vmax条件下,每摩尔与酶结合的黄素的周转数为1600/分钟。与酶结合的黄素的光谱因S-腺苷甲硫氨酸的结合而受到显著干扰,S-腺苷甲硫氨酸是一种已知为该酶变构调节剂的代谢物。