Brocklehurst K, Malthouse J P, Shipton M
Biochem J. 1979 Nov 1;183(2):223-31. doi: 10.1042/bj1830223.
A method is proposed by which site-specific reactivity probes that exhibit different reactivities in two ionization states can be used to detect association-activation phenomena that involve repositioning of acid/base groups in enzyme active centres. The pH-dependences of the apparent second-order rate constants (k) for the reactions of the thiol group of papain (EC 3.4.22.2) with a series of two-protonic-state reactivity probes are compared. The short-chain probes, 2,2'-dipyridyl disulphide and n-propyl 2-pyridyl disulphide, react at pH6 in adsorptive complexes and/or transition states with geometries that do not permit hydrogen-bonding of the pyridyl nitrogen atom with the active-centre imidazolium ion, as evidenced by the rate minima at pH6 and the rate maxima at pH4 provided by reagent protonation. Only when the probe molecule, e.g. 4-(N-aminoethyl 2'-pyridyl disulphide)-7-nitrobenzo-2-oxa-1,3-diazole [compound(III)], contains a long hydrophobic side chain is the reaction characterized by maximal rates at about pH6, as in the acylation step of the catalytic act (at pH6, k(compound III)/k(2,2'-dipyridyl disulphide) approximately 100). It is proposed that this striking difference in profile shape may result from binding of the hydrophobic side chain of compound (III) possibly in the S(2)-subsite of papain, which promotes a change in catalytic-site geometry involving repositioning of the imidazolium ion of histidine-159 and hydrogen-bonding with the N atom of the leaving group, as has been postulated to occur in the acylation step of substate hydrolysis.
本文提出了一种方法,通过该方法可利用在两种电离状态下表现出不同反应活性的位点特异性反应探针,来检测涉及酶活性中心酸碱基团重新定位的缔合-活化现象。比较了木瓜蛋白酶(EC 3.4.22.2)的巯基与一系列双质子态反应探针反应的表观二级速率常数(k)的pH依赖性。短链探针2,2'-二吡啶二硫化物和正丙基2-吡啶二硫化物在pH6时于吸附复合物和/或过渡态中反应,其几何结构不允许吡啶氮原子与活性中心咪唑离子形成氢键,这由pH6时的速率最小值和试剂质子化提供的pH4时的速率最大值证明。只有当探针分子,例如4-(N-氨基乙基2'-吡啶二硫化物)-7-硝基苯并-2-恶唑-1,3-二唑[化合物(III)]含有长疏水侧链时,反应才表现出在约pH6时的最大速率,如同催化作用的酰化步骤(在pH6时,k(化合物III)/k(2,2'-二吡啶二硫化物)约为100)。有人提出,这种显著的曲线形状差异可能是由于化合物(III)的疏水侧链可能结合在木瓜蛋白酶的S(2)亚位点上,这促进了催化位点几何结构的变化,涉及组氨酸-159的咪唑离子重新定位并与离去基团的N原子形成氢键,正如在底物水解的酰化步骤中所推测发生的那样。