Department of Biochemistry, University of Texas Southwestern Medical Center at Dallas, Dallas, Texas 75390-9038, USA.
J Biol Chem. 2012 Mar 16;287(12):9178-92. doi: 10.1074/jbc.M111.314963. Epub 2012 Jan 30.
The branched-chain α-ketoacid dehydrogenase phosphatase (BDP) component of the human branched-chain α-ketoacid dehydrogenase complex (BCKDC) has been expressed in Escherichia coli and purified in the soluble form. The monomeric BDP shows a strict dependence on Mn(2+) ions for phosphatase activity, whereas Mg(2+) and Ca(2+) ions do not support catalysis. Metal binding constants for BDP, determined by competition isothermal titration calorimetry, are 2.4 nm and 10 μm for Mn(2+) and Mg(2+) ions, respectively. Using the phosphorylated decarboxylase component (p-E1b) of BCKDC as a substrate, BDP shows a specific activity of 68 nmol/min/mg. The Ca(2+)-independent binding of BDP to the 24-meric transacylase (dihydrolipoyl transacylase; E2b) core of BCKDC results in a 3-fold increase in the dephosphorylation rate of p-E1b. However, the lipoyl prosthetic group on E2b is not essential for BDP binding or E2b-stimulated phosphatase activity. Acidic residues in the C-terminal linker of the E2b lipoyl domain are essential for the interaction between BDP and E2b. The BDP structure was determined by x-ray crystallography to 2.4 Å resolution. The BDP structure is dominated by a central β-sandwich. There are two protrusions forming a narrow cleft ∼10 Å wide, which constitutes the active site. The carboxylate moieties of acidic residues Asp-109, Asp-207, Asp-298, and Asp-337 in the active-site cleft participate in binding two metal ions. Substitutions of these residues with alanine nullify BDP phosphatase activity. Alteration of the nearby Arg-104 increases the K(m) for p-E1b peptide by 60-fold, suggesting that this residue is critical for the recognition of the native p-E1b protein.
人支链α-酮酸脱氢酶复合物(BCKDC)的支链α-酮酸脱氢酶磷酸酶(BDP)已在大肠杆菌中表达并以可溶性形式纯化。单体 BDP 显示出对磷酸酶活性的严格依赖性Mn(2+)离子,而 Mg(2+)和 Ca(2+)离子不支持催化。通过竞争等温滴定量热法测定的 BDP 的金属结合常数分别为 2.4nm 和 10μm。使用 BCKDC 的磷酸化脱羧酶组件(p-E1b)作为底物,BDP 的比活性为 68nmol/min/mg。BDP 与 BCKDC 的 24 聚转酰酶(二氢硫辛酸转酰酶;E2b)核心的 Ca(2+)独立结合导致 p-E1b 的去磷酸化速率增加 3 倍。然而,E2b 上的脂酰辅基对于 BDP 结合或 E2b 刺激的磷酸酶活性不是必需的。E2b 脂酰结构域的 C 末端接头中的酸性残基对于 BDP 和 E2b 之间的相互作用是必需的。通过 X 射线晶体学将 BDP 结构确定为 2.4Å分辨率。BDP 结构主要由中心β-夹心组成。有两个突起形成一个约 10Å宽的狭窄裂缝,构成活性位点。活性位点裂缝中的酸性残基 Asp-109、Asp-207、Asp-298 和 Asp-337 的羧基部分参与结合两个金属离子。这些残基的丙氨酸取代使 BDP 磷酸酶活性丧失。附近的 Arg-104 取代增加了 p-E1b 肽的 K(m)值 60 倍,表明该残基对于识别天然 p-E1b 蛋白至关重要。