Matulis Daumantas, Kranz James K, Salemme F Raymond, Todd Matthew J
Johnson & Johnson Pharmaceutical Research & Development, LLC, Eagleview Corporate Center, 665 Stockton Drive, Suite 104, Exton, Pennsylvania 19341, USA.
Biochemistry. 2005 Apr 5;44(13):5258-66. doi: 10.1021/bi048135v.
ThermoFluor (a miniaturized high-throughput protein stability assay) was used to analyze the linkage between protein thermal stability and ligand binding. Equilibrium binding ligands increase protein thermal stability by an amount proportional to the concentration and affinity of the ligand. Binding constants (K(b)) were measured by examining the systematic effect of ligand concentration on protein stability. The precise ligand effects depend on the thermodynamics of protein stability: in particular, the unfolding enthalpy. An extension of current theoretical treatments was developed for tight binding inhibitors, where ligand effect on T(m) can also reveal binding stoichiometry. A thermodynamic analysis of carbonic anhydrase by differential scanning calorimetry (DSC) enabled a dissection of the Gibbs free energy of stability into enthalpic and entropic components. Under certain conditions, thermal stability increased by over 30 degrees C; the heat capacity of protein unfolding was estimated from the dependence of calorimetric enthalpy on T(m). The binding affinity of six sulfonamide inhibitors to two isozymes (human type 1 and bovine type 2) was analyzed by both ThermoFluor and isothermal titration calorimetry (ITC), resulting in a good correlation in the rank ordering of ligand affinity. This combined investigation by ThermoFluor, ITC, and DSC provides a detailed picture of the linkage between ligand binding and protein stability. The systematic effect of ligands on stability is shown to be a general tool to measure affinity.
热荧光法(一种小型化高通量蛋白质稳定性测定方法)用于分析蛋白质热稳定性与配体结合之间的联系。平衡结合配体可使蛋白质热稳定性提高,提高的幅度与配体的浓度和亲和力成正比。通过研究配体浓度对蛋白质稳定性的系统性影响来测量结合常数(K(b))。精确的配体效应取决于蛋白质稳定性的热力学性质,特别是去折叠焓。针对紧密结合抑制剂开发了当前理论处理方法的扩展,其中配体对T(m)的影响也可揭示结合化学计量。通过差示扫描量热法(DSC)对碳酸酐酶进行热力学分析,能够将稳定性的吉布斯自由能分解为焓和熵成分。在某些条件下,热稳定性提高超过30摄氏度;根据量热焓对T(m)的依赖性估算蛋白质去折叠的热容。通过热荧光法和等温滴定量热法(ITC)分析了六种磺胺类抑制剂对两种同工酶(人1型和牛2型)的结合亲和力,结果在配体亲和力的排序上具有良好的相关性。热荧光法、ITC和DSC的这种联合研究提供了配体结合与蛋白质稳定性之间联系的详细情况。配体对稳定性的系统性影响被证明是测量亲和力的通用工具。