Gagné S M, Tsuda S, Li M X, Chandra M, Smillie L B, Sykes B D
Department of Biochemistry, University of Alberta, Edmonton, Canada.
Protein Sci. 1994 Nov;3(11):1961-74. doi: 10.1002/pro.5560031108.
The backbone resonance assignments have been completed for the apo (1H and 15N) and calcium-loaded (1H, 15N, and 13C) regulatory N-domain of chicken skeletal troponin-C (1-90), using multidimensional homonuclear and heteronuclear NMR spectroscopy. The chemical-shift information, along with detailed NOE analysis and 3JHNH alpha coupling constants, permitted the determination and quantification of the Ca(2+)-induced secondary structural change in the N-domain of TnC. For both structures, 5 helices and 2 short beta-strands were found, as was observed in the apo N-domain of the crystal structure of whole TnC (Herzberg O, James MNG, 1988, J Mol Biol 203:761-779). The NMR solution structure of the apo form is indistinguishable from the crystal structure, whereas some structural differences are evident when comparing the 2Ca2+ state solution structure with the apo one. The major conformational change observed is the straightening of helix-B upon Ca2+ binding. The possible importance and role of this conformational change is explored. Previous CD studies on the regulatory domain of TnC showed a significant Ca(2+)-induced increase in negative ellipticity, suggesting a significant increase in helical content upon Ca2+ binding. The present study shows that there is virtually no change in alpha-helical content associated with the transition from apo to the 2Ca2+ state of the N-domain of TnC. Therefore, the Ca(2+)-induced increase in ellipticity observed by CD does not relate to a change in helical content, but more likely to changes in spatial orientation of helices.
利用多维同核和异核核磁共振光谱,已完成对鸡骨骼肌肌钙蛋白C(1-90)的脱辅基(1H和15N)及钙负载(1H、15N和13C)调节性N结构域的主链共振归属。化学位移信息,连同详细的NOE分析和3JHNHα耦合常数,使得能够确定和量化TnC的N结构域中Ca(2+)诱导的二级结构变化。对于这两种结构,均发现了5个螺旋和2条短β链,这与完整TnC晶体结构的脱辅基N结构域中观察到的情况相同(Herzberg O,James MNG,1988,J Mol Biol 203:761-779)。脱辅基形式的NMR溶液结构与晶体结构无法区分,而将2Ca2+状态的溶液结构与脱辅基结构进行比较时,一些结构差异很明显。观察到的主要构象变化是Ca2+结合后螺旋B伸直。探讨了这种构象变化可能的重要性和作用。先前对TnC调节结构域的CD研究表明,Ca(2+)诱导负椭圆率显著增加,表明Ca2+结合后螺旋含量显著增加。本研究表明,TnC的N结构域从脱辅基状态转变为2Ca2+状态时,α螺旋含量几乎没有变化。因此,CD观察到的Ca(2+)诱导的椭圆率增加与螺旋含量的变化无关,而更可能与螺旋空间取向的变化有关。