Department of Biochemistry, Case Western Reserve University, 10900 Euclid Avenue, Cleveland, Ohio 44106, USA.
J Am Chem Soc. 2012 Oct 10;134(40):16798-804. doi: 10.1021/ja3073676. Epub 2012 Sep 26.
The rise of inhibitor-resistant and other β-lactamase variants is generating an interest in developing new β-lactamase inhibitors to complement currently available antibiotics. To gain insight into the chemistry of inhibitor recognition, we determined the crystal structure of the inhibitor preacylation complex of sulbactam, a clinical β-lactamase inhibitor, bound in the active site of the S70C variant of SHV-1 β-lactamase, a resistance enzyme that is normally present in Klebsiella pneumoniae. The S70C mutation was designed to affect the reactivity of that catalytic residue to allow for capture of the preacylation complex. Unexpectedly, the 1.45 Å resolution inhibitor complex structure revealed that residue C70 is involved in a sulfenamide bond with K73. Such a covalent bond is not present in the wild-type SHV-1 or in an apo S70C structure also determined in this study. This bond likely contributed significantly to obtaining the preacylation complex with sulbactam due to further decreased reactivity toward substrates. The intact sulbactam is positioned in the active site such that its carboxyl moiety interacts with R244, S130, and T235 and its carbonyl moiety is situated in the oxyanion hole. To our knowledge, in addition to being the first preacylation inhibitor β-lactamase complex, this is also the first observation of a sulfenamide bond between a cysteine and lysine in an active site. Not only could our results aid, therefore, structure-based inhibitor design efforts in class A β-lactamases, but the sulfenamide-bond forming approach to yield preacylation complexes could also be applied to other classes of β-lactamases and penicillin-binding proteins with the SXXK motif.
抑制剂耐药性和其他β-内酰胺酶变体的出现,促使人们开发新的β-内酰胺酶抑制剂来补充现有的抗生素。为了深入了解抑制剂识别的化学原理,我们测定了舒巴坦(一种临床用β-内酰胺酶抑制剂)酰化前复合物与 SHV-1β-内酰胺酶 S70C 变体的活性部位结合的晶体结构,SHV-1β-内酰胺酶是一种耐药酶,通常存在于肺炎克雷伯氏菌中。S70C 突变旨在影响该催化残基的反应性,从而捕获酰化前复合物。出乎意料的是,在 1.45Å分辨率的抑制剂复合物结构中发现,残基 C70 与 K73 形成了磺酰胺键。这种共价键在野生型 SHV-1 或本研究中也确定的 apo S70C 结构中并不存在。由于对底物的反应性进一步降低,这种键可能对获得与舒巴坦的酰化前复合物有显著贡献。完整的舒巴坦被定位在活性部位,使其羧基部分与 R244、S130 和 T235 相互作用,其羰基部分位于氧阴离子穴中。据我们所知,除了是第一个酰化前抑制剂β-内酰胺酶复合物外,这也是首次在活性部位观察到半胱氨酸和赖氨酸之间形成磺酰胺键。因此,我们的结果不仅可以帮助基于结构的抑制剂设计工作在 A 类β-内酰胺酶中,而且形成磺酰胺键的方法也可以应用于具有 SXXK 基序的其他类β-内酰胺酶和青霉素结合蛋白,以产生酰化前复合物。