Zanardelli Sara, Crawley James T B, Chion Chan K N Chan Kwo, Lam Jonathan K, Preston Roger J S, Lane David A
Department of Haematology, Imperial College London, London W12 ONN, United Kingdom.
J Biol Chem. 2006 Jan 20;281(3):1555-63. doi: 10.1074/jbc.M508316200. Epub 2005 Oct 12.
ADAMTS13 controls the multimeric size of circulating von Willebrand factor (VWF) by cleaving the Tyr1605-Met1606 bond in theA2 domain. To examine substrate recognition, we expressed in bacteria and purified three A2 (VWF76-(1593-1668), VWF115-(1554-1668), VWFA2-(1473-1668)) and one A2-A3 (VWF115-A3-(1554-1874)) domain fragments. Using high pressure liquid chromatography analysis, the initial rates of VWF115 cleavage by ADAMTS13 at different substrate concentrations were determined, and from this the kinetic constants were derived (Km 1.61 microM; kcat 0.14 s(-1)), from which the specificity constant kcat/Km was calculated, 8.70 x 10(4) m(-1) s(-1). Similar values of the specificity constant were obtained for VWF76 and VWF115-A3. To identify residues important for recognition and proteolysis of VWF115, we introduced certain type 2A von Willebrand disease mutations by site-directed mutagenesis. Although most were cleaved normally, one (D1614G) was cleaved approximately 8-fold slower. Mutagenesis of additional charged residues predicted to be in close proximity to Asp1614 on the surface of the A2 domain (R1583A, D1587A, D1614A, E1615A, K1617A, E1638A, E1640A) revealed up to 13-fold reduction in kcat/Km for D1587A, D1614A, E1615A, and K1617A mutants. When introduced into the intact VWFA2 domain, proteolysis of the D1587A, D1614A, and E1615A mutants was also slowed, particularly in the presence of urea. Surface plasmon resonance demonstrated appreciable reduction in binding affinity between ADAMTS13 and VWF115 mutants (KD up to approximately 1.3 microM), compared with VWF115 (KD 20 nM). These results demonstrate an important role for Asp1614 and surrounding charged residues in the binding and cleavage of the VWFA2 domain by ADAMTS13.
ADAMTS13 通过切割 A2 结构域中的 Tyr1605-Met1606 键来控制循环血管性血友病因子(VWF)的多聚体大小。为了研究底物识别,我们在细菌中表达并纯化了三个 A2(VWF76-(1593 - 1668)、VWF115-(1554 - 1668)、VWFA2-(1473 - 1668))和一个 A2-A3(VWF115-A3-(1554 - 1874))结构域片段。使用高压液相色谱分析,测定了在不同底物浓度下 ADAMTS13 切割 VWF115 的初始速率,并由此推导出动力学常数(Km 1.61 microM;kcat 0.14 s(-1)),据此计算出特异性常数 kcat/Km 为 8.70 x 10(4) m(-1) s(-1)。VWF76 和 VWF115-A3 也获得了相似的特异性常数值。为了确定对 VWF115 的识别和蛋白水解重要的残基,我们通过定点诱变引入了某些 2A 型血管性血友病疾病突变。尽管大多数突变体被正常切割,但其中一个(D1614G)的切割速度慢了约 8 倍。对 A2 结构域表面预计与 Asp1614 紧邻的其他带电残基(R1583A、D1587A、D1614A、E1615A、K1617A、E1638A、E1640A)进行诱变后发现,D1587A、D1614A、E1615A 和 K1617A 突变体的 kcat/Km 降低了高达 13 倍。当引入完整的 VWFA2 结构域时,D1587A、D1614A 和 E1615A 突变体的蛋白水解也减慢,尤其是在有尿素存在的情况下。表面等离子体共振表明,与 VWF115(KD 20 nM)相比,ADAMTS13 与 VWF115 突变体之间的结合亲和力明显降低(KD 高达约 1.3 microM)。这些结果表明 Asp1614 和周围带电残基在 ADAMTS13 对 VWFA2 结构域的结合和切割中起重要作用。