Huang Yu-chu, Misquitta Stephanie, Blond Sylvie Y, Adams Elizabeth, Colman Roberta F
Department of Chemistry and Biochemistry, University of Delaware, Newark, Delaware 19716, USA.
J Biol Chem. 2008 Nov 21;283(47):32880-8. doi: 10.1074/jbc.M805484200. Epub 2008 Sep 16.
Human glutathione transferase pi (GST pi) has been crystallized as a homodimer, with a subunit molecular mass of approximately 23 kDa; however, in solution the average molecular mass depends on protein concentration, approaching that of monomer at <0.03 mg/ml, concentrations typically used to measure catalytic activity of the enzyme. Electrostatic interaction at the subunit interface greatly influences the dimer-monomer equilibrium of the enzyme and is an important force for holding subunits together. Arg-70, Arg-74, Asp-90, Asp-94, and Thr-67 were selected as target sites for mutagenesis, because they are at the subunit interface. R70Q, R74Q, D90N, D94N, and T67A mutant enzymes were constructed, expressed in Escherichia coli, and purified. The construct of N-terminal His tag enzyme facilitates the purification of GST pi, resulting in a high yield of enzyme, but does not alter the kinetic parameters or secondary structure of the enzyme. Our results indicate that these mutant enzymes show no appreciable changes in K(m) for 1-chloro-2,4-dinitrobenzene and have similar CD spectra to that of wild-type enzyme. However, elimination of the charges of either Arg-70, Arg-74, Asp-90, or Asp-94 shifts the dimer-monomer equilibrium toward monomer. In addition, replacement of Asp-94 or Arg-70 causes a large increase in the K(m)(GSH), whereas substitution for Asp-90 or Arg-74 primarily results in a marked decrease in V(max). The GST pi retains substantial catalytic activity as a monomer probably because the glutathione and electrophilic substrate sites (such as for 1-chloro-2,4-dinitrobenzene) are predominantly located within each subunit.
人谷胱甘肽转移酶π(GST π)已结晶为同二聚体,亚基分子量约为23 kDa;然而,在溶液中,平均分子量取决于蛋白质浓度,在<0.03 mg/ml(通常用于测量该酶催化活性的浓度)时接近单体分子量。亚基界面处的静电相互作用极大地影响了该酶的二聚体 - 单体平衡,是将亚基维系在一起的重要力量。选择Arg - 70、Arg - 74、Asp - 90、Asp - 94和Thr - 67作为诱变的靶位点,因为它们位于亚基界面。构建了R70Q、R74Q、D90N、D94N和T67A突变酶,在大肠杆菌中表达并纯化。N端His标签酶的构建有助于GST π的纯化,可实现该酶的高产率,但不会改变酶的动力学参数或二级结构。我们的结果表明,这些突变酶对1 - 氯 - 2,4 - 二硝基苯的K(m)没有明显变化,并且具有与野生型酶相似的圆二色光谱。然而,消除Arg - 70、Arg - 74、Asp - 90或Asp - 94中的任何一个电荷会使二聚体 - 单体平衡向单体方向移动。此外,Asp - 94或Arg - 70的替换导致K(m)(GSH)大幅增加,而Asp - 90或Arg - 74的替换主要导致V(max)显著降低。GST π作为单体保留了大量催化活性,可能是因为谷胱甘肽和亲电底物位点(如对于1 - 氯 - 2,4 - 二硝基苯)主要位于每个亚基内。