Department of Chemistry, Portland State University , Portland, Oregon 97207-0751, United States.
Chem Res Toxicol. 2013 Jan 18;26(1):112-23. doi: 10.1021/tx300417z. Epub 2012 Dec 27.
Benzoquinone (BQ) is an extremely potent electrophilic contact allergen that haptenates endogenous proteins through Michael addition (MA). It is also hypothesized that BQ may haptenate proteins via free radical formation. The objective of this study was to assess the inductive effects (activating and deactivating) of substituents on BQ reactivity and the mechanistic pathway of covalent binding to a nucleophilic thiol. The BQ binding of Cys34 on human serum albumin was studied, and for reactivity studies, nitrobenzenethiol (NBT) was used as a surrogate for protein binding of the BQ and benzoquinone derivatives (BQD). Stopped flow techniques were used to determine pseudofirst order rate constants (k) of methyl-, t-butyl-, and chlorine-substituted BQD reactions with NBT, whereas electron pair resonance (EPR) studies were performed to investigate the presence of the free radical mediated binding mechanism of BQD. Characterization of adducts was performed using mass spectrometry and nuclear magnetic resonance spectroscopy (NMR). The rate constant values demonstrated the chlorine-substituted (activated) BQD to be more reactive toward NBT than the methyl and t-butyl-substituted (deactivated) BQD, and this correlated with the respective EPR intensities. The EPR signal, however, was quenched in the presence of NBT suggesting MA as the dominant reaction pathway. MS and NMR results confirmed adduct formation to be a result of MA onto the BQ ring with vinylic substitution also occurring for chlorine-substituted derivatives. The binding positions on BQ and NBT/BQ(D) stoichiometric ratios were affected by whether the inductive effects of the substituents on the ring were positive or negative. The reactivity of BQ and BQD is discussed in terms of the potential relationship to potential allergenic potency.
苯醌(BQ)是一种极其有效的亲电接触过敏原,通过迈克尔加成(MA)使内源性蛋白加合物化。也有人假设 BQ 可能通过自由基形成使蛋白质加合物化。本研究的目的是评估取代基对 BQ 反应性的诱导效应(激活和失活),以及与亲核巯基共价结合的机制途径。研究了 BQ 在人血清白蛋白上与半胱氨酸残基 34 的结合,并且对于反应性研究,使用硝基苯硫醇(NBT)作为 BQ 和苯醌衍生物(BQD)与蛋白质结合的替代物。使用停流技术确定了 NBT 与甲基、叔丁基和氯取代的 BQD 反应的假一级速率常数(k),而电子对共振(EPR)研究则用于研究 BQD 的自由基介导结合机制的存在。使用质谱和核磁共振光谱(NMR)对加合物进行了表征。速率常数值表明,氯取代(激活)的 BQD 比甲基和叔丁基取代(失活)的 BQD 对 NBT 的反应性更强,这与相应的 EPR 强度相关。然而,EPR 信号在存在 NBT 时被猝灭,这表明 MA 是主要的反应途径。MS 和 NMR 结果证实,加合物的形成是由于 BQ 环上的 MA,并且对于氯取代的衍生物也发生了烯键取代。BQ 和 NBT/BQ(D)的结合位置受到取代基对环的诱导效应是正还是负的影响。根据 BQ 和 BQD 的潜在反应性,讨论了它们与潜在致敏性的关系。