Tremblay J M, Li H, Yarbrough L R, Helmkamp G M
Department of Biochemistry and Molecular Biology, University of Kansas Medical Center, Kansas City, Kansas 66160-7421, USA.
Biochemistry. 2001 Aug 7;40(31):9151-8. doi: 10.1021/bi0107896.
The alpha isoforms of mammalian phosphatidylinositol transfer protein (PITP) contain four conserved Cys residues. In this investigation, a series of thiol-modifying reagents, both alkylating and mixed disulfide-forming, was employed to define the accessibility of these residues and to evaluate their role in protein-mediated intermembrane phospholipid transport. Isolation and analysis of chemically modified peptides and site-directed mutagenesis of each Cys residue to Ala were also performed. Soluble, membrane-associated, and denatured preparations of wild-type and mutant rat PITPs were studied. Under denaturing conditions, all four Cys residues could be detected spectrophotometrically by chemical reaction with 4,4'-dipyridyl disulfide or 5,5'-dithiobis(2-nitrobenzoate). In the native protein, two of the four Cys residues were sensitive to some but not all thiol-modifying reagents, with discrimination based on the charge and hydrophobicity of the reagent and the conformation of the protein. With the soluble conformation of PITP, achieved in the absence of phospholipid vesicles, the surface-exposed Cys(188) was chemically modified without consequence to lipid transfer activity. Cys(188) exhibited an apparent pK(a) of 7.6. The buried Cys(95), which constitutes part of the phospholipid substrate binding site, was covalently modified upon transient association of PITP with a membrane surface. The Cys-to-Ala mutations showed that neither Cys(95) nor Cys(188) was essential for lipid transfer activity. However, chemical modification of Cys(95) resulted in the loss of lipid transfer activity. These results demonstrate that the Cys residues of PITP can be assigned to several different classes of chemical reactivity. Of particular interest is Cys(95), whose sulfhydryl group becomes exposed to modification in the membrane-associated conformation of PITP. Furthermore, the inhibition of PITP activity by thiol-modifying reagents is a result of steric hindrance of phospholipid substrate binding.
哺乳动物磷脂酰肌醇转移蛋白(PITP)的α亚型含有四个保守的半胱氨酸残基。在本研究中,使用了一系列硫醇修饰试剂,包括烷基化试剂和形成混合二硫键的试剂,来确定这些残基的可及性,并评估它们在蛋白质介导的膜间磷脂转运中的作用。还进行了化学修饰肽的分离和分析以及每个半胱氨酸残基到丙氨酸的定点诱变。研究了野生型和突变型大鼠PITP的可溶性、膜相关和变性制剂。在变性条件下,通过与4,4'-二吡啶二硫化物或5,5'-二硫代双(2-硝基苯甲酸)的化学反应,可以用分光光度法检测到所有四个半胱氨酸残基。在天然蛋白质中,四个半胱氨酸残基中的两个对某些但不是所有硫醇修饰试剂敏感,这取决于试剂的电荷和疏水性以及蛋白质的构象。在没有磷脂囊泡的情况下实现PITP的可溶性构象时,表面暴露的半胱氨酸(188)被化学修饰,而脂质转移活性不受影响。半胱氨酸(188)的表观pK(a)为7.6。构成磷脂底物结合位点一部分的埋藏半胱氨酸(95)在PITP与膜表面短暂结合时被共价修饰。半胱氨酸到丙氨酸的突变表明,半胱氨酸(95)和半胱氨酸(188)对脂质转移活性都不是必需的。然而,半胱氨酸(95)的化学修饰导致脂质转移活性丧失。这些结果表明,PITP的半胱氨酸残基可以分为几种不同的化学反应类别。特别有趣的是半胱氨酸(95),其巯基在PITP的膜相关构象中变得易于修饰。此外,硫醇修饰试剂对PITP活性的抑制是磷脂底物结合的空间位阻的结果。