Department of Chemistry, University of Georgia, Athens, GA, United States.
Department of Chemistry, University of Georgia, Athens, GA, United States.
Methods Enzymol. 2024;704:3-25. doi: 10.1016/bs.mie.2024.05.020. Epub 2024 Jun 8.
Extradiol dioxygenases are a class of non-heme iron-dependent enzymes found in eukaryotes and prokaryotes that play a vital role in the aerobic catabolism of aromatic compounds. They are generally divided into three evolutionarily independent superfamilies with different protein folds. Our recent studies have shed light on the catalytic mechanisms and structure-function relationships of two specific extradiol dioxygenases: 3-hydroxyanthranilate-3,4-dioxygenase, a Type III enzyme essential in mammals for producing a precursor for nicotinamide adenine dinucleotide, and L-3,4-dihydroxyphenylalanine dioxygenase, an uncommon form of Type I enzymes involved in natural product biosynthesis. This work details the expression and isolation methods for these extradiol dioxygenases and introduces approaches to achieve homogeneity and high occupancy of the enzyme metal centers. Techniques such as ultraviolet-visible and electron paramagnetic resonance spectroscopies, as well as oxygen electrode measurements, are discussed for probing the interaction of the non-heme iron center with ligands and characterizing enzymatic activities. Moreover, protein crystallization has been demonstrated as a powerful tool to study these enzymes. We highlight in crystallo reactions and single-crystal spectroscopic methods to further elucidate enzymatic functions and protein dynamics.
外二醇双加氧酶是一类存在于真核生物和原核生物中的非血红素铁依赖性酶,在芳香族化合物的需氧分解中起着至关重要的作用。它们通常分为三个在进化上独立的超家族,具有不同的蛋白质折叠。我们最近的研究揭示了两种特定的外二醇双加氧酶的催化机制和结构功能关系:3-羟邻氨基苯甲酸-3,4-双加氧酶,这是哺乳动物中产生烟酰胺腺嘌呤二核苷酸前体所必需的 III 型酶;L-3,4-二羟基苯丙氨酸双加氧酶,这是一种参与天然产物生物合成的不常见的 I 型酶。这项工作详细介绍了这些外二醇双加氧酶的表达和分离方法,并介绍了实现酶金属中心均匀性和高占有率的方法。讨论了紫外可见和电子顺磁共振波谱以及氧电极测量等技术,用于探测非血红素铁中心与配体的相互作用并表征酶活性。此外,蛋白质结晶已被证明是研究这些酶的有力工具。我们强调了在结晶反应和单晶光谱方法中进一步阐明酶功能和蛋白质动力学。