Okumura Nobuaki, Tamura Jun, Takao Toshifumi
Laboratory of Homeostatic Integration, Institute for Protein Research, Osaka University, Suita, Osaka, 565-0871, Japan.
Mass Spectrometry Business Unit, JEOL Ltd, Akishima, Tokyo, 196-8558, Japan.
Protein Sci. 2016 Feb;25(2):511-22. doi: 10.1002/pro.2842. Epub 2015 Nov 25.
Carnosine dipeptidase II (CN2/CNDP2) is an M20 family metallopeptidase that hydrolyses various dipeptides including β-alanyl-L-histidine (carnosine). Crystallographic analysis showed that CN2 monomer is composed of one catalytic and one dimerization domains, and likely to form homodimer. In this crystal, H228 residue of the dimerization domain interacts with the substrate analogue bestatin on the active site of the dimer counterpart, indicating that H228 is involved in enzymatic reaction. In the present study, the role of intradimer interaction of CN2 in its catalytic activity was investigated using electrospray-ionization time-of-flight mass spectrometry (ESI-TOF MS). First, a dimer interface mutant I319K was prepared and shown to be present as a folded monomer in solution as examined by using ESI-TOF MS. Since the mutant was inactive, it was suggested that dimer formation is essential to its enzymatic activity. Next, we prepared H228A and D132A mutant proteins with different N-terminal extended sequences, which enabled us to monitor dimer exchange reaction by ESI-TOF MS. The D132A mutant is a metal ligand mutant and also inactive. But the activity was partially recovered time-dependently when H228A and D132A mutant proteins were incubated together. In parallel, H228A/D132A heterodimer was formed as detected by ESI-TOF MS, indicating that interaction of a catalytic center with H228 residue of the other subunit is essential to the enzymatic reaction. These results provide evidence showing that intradimer interaction of H228 with the reaction center of the dimer counterpart is essential to the enzymatic activity of CN2.
肌肽二肽酶II(CN2/CNDP2)是一种M20家族金属肽酶,可水解包括β-丙氨酰-L-组氨酸(肌肽)在内的多种二肽。晶体学分析表明,CN2单体由一个催化结构域和一个二聚化结构域组成,可能形成同源二聚体。在该晶体中,二聚化结构域的H228残基与二聚体对应物活性位点上的底物类似物苯丁抑制素相互作用,表明H228参与酶促反应。在本研究中,使用电喷雾电离飞行时间质谱(ESI-TOF MS)研究了CN2二聚体内相互作用在其催化活性中的作用。首先,制备了二聚体界面突变体I319K,通过ESI-TOF MS检测表明其在溶液中以折叠单体形式存在。由于该突变体无活性,提示二聚体形成对其酶活性至关重要。接下来,我们制备了具有不同N端延伸序列的H228A和D132A突变蛋白,这使我们能够通过ESI-TOF MS监测二聚体交换反应。D132A突变体是一种金属配体突变体,也无活性。但当H228A和D132A突变蛋白一起孵育时,活性随时间部分恢复。同时,ESI-TOF MS检测到形成了H228A/D132A异二聚体,表明一个催化中心与另一个亚基的H228残基相互作用对酶促反应至关重要。这些结果提供了证据,表明H228与二聚体对应物反应中心的二聚体内相互作用对CN2的酶活性至关重要。