Herberg F W, Zimmermann B, McGlone M, Taylor S S
Abt. für Biochemie Supramolekularer Systeme, Ruhr-Universität Bochum, Germany.
Protein Sci. 1997 Mar;6(3):569-79. doi: 10.1002/pro.5560060306.
All eukaryotic protein kinases share a conserved catalytic core. In the catalytic (C) subunit of cAMP-dependent protein kinase (cAPK) this core is preceded by a myristylation motif followed by a long helix with Trp 30 at the end of this A-helix filling a hydrophobic cavity between the two lobes of the core. To understand the importance of the A-helix, the myristylation motif (delta 1-14) as well as the entire N-terminal segment (delta 1 -39) were deleted. In addition, Trp 30 was replaced with both Tyr and Ala. All proteins were overexpressed in E. coli and purified to homogeneity. rC(delta 1-14), rC(W30Y), and rC(W30A) all had reduced thermostability, but were catalytically indistinguishable from wild-type C. Based on Surface Plasmon Resonance, all three also formed stable holoenzyme complexes with the RI-subunit, although the appKds were reduced by more than 10-fold due to decrease in the association rate. Surprisingly, however, the holoenzymes were even more thermostable than wild-type holoenzyme. To obtain active enzyme, it was necessary to purify rC(delta 1-39) as a fusion protein with glutathione-S-transferase (GST-rC(delta 1-39), although its thermostability (Tm) was decreased by 12.5 degrees C, was catalytically similar to wild-type C and was inhibited by both the type I and II R-subunits and the heat-stable protein kinase inhibitor (PKI). The Tm for holoenzyme II formed with GST-rC(delta 1-39) was 16.5 degrees C greater than the Tm for free GST-rC(delta 1-39), and the Ka(cAMP) was increased nearly 10-fold. These mutants point out striking and unanticipated differences in how the RI and RII subunits associate with the C-subunit to form a stable holoenzyme and indicate, furthermore, that this N-terminal segment, far from the active site cleft, influences those interactions. The importance of the A-helix and Trp 30 for stability correlates with its location at the cleft interface where it orients the C-helix in the small lobe and the activation loop in the large so that these subdomains are aligned in a way that allows for correct configuration of residues at the active site. This extensive network of contacts that links the A-helix directly to the active site in cAPK is compared to other kinases whose crystal structures have been solved.
所有真核生物蛋白激酶都共享一个保守的催化核心。在环磷酸腺苷依赖性蛋白激酶(cAPK)的催化(C)亚基中,这个核心之前有一个肉豆蔻酰化基序,接着是一个长螺旋,在这个A螺旋末端的色氨酸30填充了核心两个叶之间的疏水腔。为了了解A螺旋的重要性,删除了肉豆蔻酰化基序(δ1 - 14)以及整个N端片段(δ1 - 39)。此外,用酪氨酸和丙氨酸取代了色氨酸30。所有蛋白质都在大肠杆菌中过表达并纯化至均一性。rC(δ1 - 14)、rC(W30Y)和rC(W30A)的热稳定性均降低,但催化活性与野生型C无差异。基于表面等离子体共振,这三种蛋白也都与RI亚基形成了稳定的全酶复合物,尽管由于结合速率降低,其解离常数(appKds)降低了10倍以上。然而,令人惊讶的是,全酶比野生型全酶更耐热。为了获得活性酶,有必要将rC(δ1 - 39)作为与谷胱甘肽 - S - 转移酶的融合蛋白进行纯化(GST - rC(δ1 - 39)),尽管其热稳定性(Tm)降低了$12.5^{\circ}C$,但其催化活性与野生型C相似,并且受到I型和II型R亚基以及热稳定蛋白激酶抑制剂(PKI)的抑制。与GST - rC(δ1 - 39)形成的全酶II的Tm比游离的GST - rC(δ1 - 39)的Tm高$16.5^{\circ}C$,并且环磷酸腺苷的解离常数(Ka(cAMP))增加了近10倍。这些突变体指出了RI和RII亚基与C亚基结合形成稳定全酶方式上惊人且意想不到的差异,并且进一步表明,这个远离活性位点裂隙的N端片段影响了这些相互作用。A螺旋和色氨酸30对稳定性的重要性与其在裂隙界面的位置相关,在该位置它使小叶中的C螺旋和大叶中的激活环定向排列,从而使这些亚结构域以一种允许活性位点残基正确构象的方式对齐。将cAPK中直接连接A螺旋与活性位点的这种广泛的接触网络与其他已解析晶体结构的激酶进行了比较。