Whitten S T, García-Moreno E B
Department of Biophysics, Johns Hopkins University, Baltimore, Maryland 21218, USA.
Biochemistry. 2000 Nov 21;39(46):14292-304. doi: 10.1021/bi001015c.
The pH dependence of stability of staphylococcal nuclease was studied with two independent equilibrium thermodynamic approaches. First, by measurement of stability in the pH range 9 to 3.5 by fluorescence-monitored denaturation with urea (Delta), GdnHCl (Delta), and heat (Delta). Second, by numerical integration of H(+) titration curves (Delta) measured potentiometrically under native (100 mM KCl) and unfolding (6.0 M GdnHCl) conditions. The pH dependence of stability described by Delta, Delta, and Delta was comparable but significantly different from the one described by Delta. The decrease in Delta between pH 9 and pH 4 was 4 kcal/mol greater than the decrease in Delta, Delta, and Delta in the same pH range. In 6 M GdnHCl, all the ionizable groups titrated with the pK(a) values of model compounds. Therefore, Delta represents the free energy difference between the native state (N) and an ensemble of unstructured, or expanded, and highly screened conformations. In contrast, the shallower pH dependence of stability described by Delta and by Delta between pH 9 and 5 was consistent with the titration of histidines with depressed, nativelike pK(a) values in the denatured state (D). These depressed pK(a) values likely reflect long-range electrostatic interactions with the other 29 basic groups and are a consequence of the compact character of the D state. The steep change in Delta and Delta at pH < 5 suggests that near pH 5 the structural and thermodynamic character of the D state shifts toward a state in which acidic residues titrate with normal pK(a) values, presumably because the electrostatic interactions with basic residues are lost, maybe as a consequence of an expansion.
采用两种独立的平衡热力学方法研究了葡萄球菌核酸酶稳定性的pH依赖性。第一,通过用尿素(Δ)、盐酸胍(Δ)和热(Δ)进行荧光监测变性,测量pH范围为9至3.5时的稳定性。第二,通过对在天然(100 mM KCl)和去折叠(6.0 M盐酸胍)条件下通过电位滴定法测量的H⁺滴定曲线(Δ)进行数值积分。由Δ、Δ和Δ描述的稳定性的pH依赖性具有可比性,但与由Δ描述的稳定性的pH依赖性显著不同。pH 9至pH 4之间Δ的降低比相同pH范围内Δ、Δ和Δ的降低大4 kcal/mol。在6 M盐酸胍中,所有可电离基团均以模型化合物的pK(a)值进行滴定。因此,Δ代表天然状态(N)与一组无结构、或伸展且高度屏蔽的构象之间的自由能差。相比之下,由Δ和在pH 9至5之间的Δ所描述的稳定性的较浅pH依赖性与变性状态(D)中具有降低的、类似天然的pK(a)值的组氨酸的滴定一致。这些降低的pK(a)值可能反映了与其他29个碱性基团的长程静电相互作用,并且是D状态紧密特征的结果。在pH < 5时,Δ和Δ的急剧变化表明,在pH接近5时,D状态的结构和热力学特征向一种状态转变,在该状态下酸性残基以正常的pK(a)值进行滴定,大概是因为与碱性残基的静电相互作用丧失了,可能是由于膨胀的结果。