Lin L N, Mason A B, Woodworth R C, Brandts J F
Department of Chemistry, University of Massachusetts, Amherst 01003.
Biochemistry. 1994 Feb 22;33(7):1881-8. doi: 10.1021/bi00173a035.
Human serum transferrin and hen ovotransferrin have been studied by differential scanning calorimetry (DSC), in an effort to quantitatively estimate the free energy of interaction of the N- and C-domains in each protein and to further understand their interaction with chelated ferric ions. In the case of serum transferrin, separate DSC transitions are observed for the two domains while only a single, coupled transition is seen for ovotransferrin. Although domain interactions are somewhat larger for ovotransferrin (-4100 cal/mol) than for serum transferrin (-3100 cal/mol), the major cause of separated transitions for serum transferrin is that the difference in intrinsic folding stability of the N- and C-domains is about 4-fold larger than for ovotransferrin. Chelated ferric ions bind strongly to each site in both proteins and produce changes in Tm by as much as 30 degrees C. When apparent binding constants are estimated from DSC results, these appear to be substantially larger than those estimated previously from equilibrium methods at low temperatures, where very long equilibrium times must be used because of slow ligand release. Although second DSC upscans on each protein show good "reversibility", downscans on serum transferrin revealed that liganded forms of the protein are in fact not in true equilibrium during upscanning, which causes Tm values during upscans to be higher than the true reversible Tm values. The likely reason for this kinetic control over unfolding is the slow release of bound ferric ions and those effects, for technical reasons, cannot be totally eliminated by lowering the scan rate.
通过差示扫描量热法(DSC)对人血清转铁蛋白和鸡卵转铁蛋白进行了研究,旨在定量估算每种蛋白质中N结构域和C结构域相互作用的自由能,并进一步了解它们与螯合铁离子的相互作用。对于血清转铁蛋白,两个结构域观察到单独的DSC转变,而卵转铁蛋白仅观察到单一的耦合转变。尽管卵转铁蛋白的结构域相互作用(-4100卡/摩尔)比血清转铁蛋白(-3100卡/摩尔)略大,但血清转铁蛋白转变分离的主要原因是N结构域和C结构域的内在折叠稳定性差异比卵转铁蛋白大4倍左右。螯合铁离子与两种蛋白质中的每个位点都紧密结合,并使熔点变化高达30℃。当根据DSC结果估算表观结合常数时,这些常数似乎比之前在低温下通过平衡方法估算的要大得多,在低温下由于配体释放缓慢,必须使用非常长的平衡时间。尽管对每种蛋白质进行的第二次DSC升温扫描显示出良好的“可逆性”,但对血清转铁蛋白的降温扫描表明,该蛋白质的配体形式在升温扫描过程中实际上并未处于真正的平衡状态,这导致升温扫描过程中的熔点值高于真正的可逆熔点值。这种对解折叠的动力学控制的可能原因是结合铁离子的缓慢释放,并且由于技术原因,通过降低扫描速率无法完全消除这些影响。