Ramachandra M, Ambudkar S V, Chen D, Hrycyna C A, Dey S, Gottesman M M, Pastan I
Laboratory of Molecular Biology, Division of Basic Sciences, National Cancer Institute, National Institutes of Health, Bethesda, Maryland 20892, USA.
Biochemistry. 1998 Apr 7;37(14):5010-9. doi: 10.1021/bi973045u.
Human P-glycoprotein (Pgp), a plasma membrane protein that confers multidrug resistance, functions as an ATP-dependent drug efflux pump. Pgp contains two ATP binding/utilization sites and exhibits ATPase activity that is stimulated in the presence of substrates and modulating agents. The mechanism of coupling of ATP hydrolysis to drug transport is not known. To understand the role of ATP hydrolysis in drug binding, it is necessary to develop methods for purifying and reconstituting Pgp that retains properties including stimulation of ATPase activity by known substrates to an extent similar to that in the native membrane. In this study, (His)6-tagged Pgp was expressed in Trichoplusia ni (High Five) cells using the recombinant baculovirus system and purified by metal affinity chromatography. Upon reconstitution into phospholipid vesicles, purified Pgp exhibited specific binding to analogues of substrates and ATP in affinity labeling experiments and displayed a high level of drug-stimulated ATPase activity (specific activity ranging from 4.5 to 6.5 micromol min-1 mg-1). The ATPase activity was inhibited by ADP in a competitive manner, and by vanadate and N-ethylmaleimide at low concentrations. Vanadate which is known to inhibit ATPase activity by trapping MgADP at the catalytic site inhibited photoaffinity labeling of Pgp with substrate analogues, [125I]iodoarylazidoprazosin and [3H]azidopine, only under ATP hydrolysis conditions. Because vanadate-trapped Pgp is known to resemble the ADP and phosphate-bound catalytic transition state, our findings indicate that ATP hydrolysis results in a conformation with reduced affinity for substrates. A catalytic transition conformation with reduced affinity would essentially result in substrate dissociation and supports a model for drug transport in which an ATP hydrolysis-induced conformational change leads to drug release toward the extracellular medium.
人P-糖蛋白(Pgp)是一种赋予多药耐药性的质膜蛋白,作为一种依赖ATP的药物外排泵发挥作用。Pgp含有两个ATP结合/利用位点,并表现出ATP酶活性,该活性在底物和调节剂存在时受到刺激。ATP水解与药物转运的偶联机制尚不清楚。为了了解ATP水解在药物结合中的作用,有必要开发纯化和重组Pgp的方法,该方法保留的特性包括已知底物对ATP酶活性的刺激程度与天然膜中相似。在本研究中,使用重组杆状病毒系统在粉纹夜蛾(High Five)细胞中表达了(His)6标记的Pgp,并通过金属亲和色谱法进行纯化。在重新组装到磷脂囊泡中后,纯化的Pgp在亲和标记实验中表现出与底物和ATP类似物的特异性结合,并显示出高水平的药物刺激的ATP酶活性(比活性范围为4.5至6.5微摩尔·分钟-1·毫克-1)。ATP酶活性受到ADP的竞争性抑制,以及低浓度钒酸盐和N-乙基马来酰亚胺的抑制。已知钒酸盐通过在催化位点捕获MgADP来抑制ATP酶活性,仅在ATP水解条件下抑制Pgp与底物类似物[125I]碘芳基叠氮哌唑嗪和[3H]叠氮平的光亲和标记。由于已知钒酸盐捕获的Pgp类似于ADP和磷酸盐结合的催化过渡态,我们的研究结果表明ATP水解导致对底物亲和力降低的构象。亲和力降低的催化过渡构象基本上会导致底物解离,并支持一种药物转运模型,其中ATP水解诱导的构象变化导致药物向细胞外介质释放。