Bordini E, Hamdan M, Righetti P G
Glaxo Wellcome Medicines Research Center, via Fleming 4, Verona, Italy.
Rapid Commun Mass Spectrom. 1999;13(18):1818-27. doi: 10.1002/(SICI)1097-0231(19990930)13:18<1818::AID-RCM723>3.0.CO;2-K.
There is compelling evidence to suggest that cysteine-acrylamide adduct formation is a modification experienced by proteins separated by two-dimensional (2-D) gel electrophoresis. Whether the -SH group involved in such complexation is offered by a free or initially disulphide-linked cysteine residue remains an open question. To address this question a number of proteins containing free and/or disulphide-linked cysteine (Cys) residues have been incubated with acrylamide monomer and examined by delayed extraction matrix-assisted laser desorption/ionisation time-of-flight (MALDI-TOF). These data provide strong evidence to suggest that the presence of free Cys in the investigated proteins is not the most important requirement for the observation of Cys-acrylamide adducts. Unambiguous confirmation of this deduction was obtained by analysing the tryptic digests of the same proteins by reflectron MALDI-TOF. The assignment of the adduction sites was facilitated by the mass accuracy attained for the monitored tryptic fragments and their agreement with the corresponding predicted masses reported in the Swiss-Prot database. The same data suggest that at high pH the cysteine pairing is flexible enough to allow initially S-S linked residues to complex with acrylamide. It is also plausible that the -NH(2) terminal blockage so often encountered in proteins electroblotted from 2-D maps could originate from carbamylation, and might not have anything to do with alkylation by free, unreacted acrylamide in polyacrylamide gels.
有确凿证据表明,半胱氨酸 - 丙烯酰胺加合物的形成是二维(2 - D)凝胶电泳分离的蛋白质所经历的一种修饰。参与这种络合作用的 -SH 基团是由游离的还是最初以二硫键连接的半胱氨酸残基提供,仍是一个悬而未决的问题。为了解决这个问题,已将一些含有游离和/或二硫键连接的半胱氨酸(Cys)残基的蛋白质与丙烯酰胺单体一起孵育,并通过延迟提取基质辅助激光解吸/电离飞行时间(MALDI - TOF)进行检测。这些数据提供了有力证据,表明在所研究的蛋白质中游离 Cys 的存在并非观察到半胱氨酸 - 丙烯酰胺加合物的最重要条件。通过反射式 MALDI - TOF 分析相同蛋白质的胰蛋白酶消化产物,得到了对这一推断的明确证实。监测的胰蛋白酶片段所达到的质量准确度及其与 Swiss - Prot 数据库中报告的相应预测质量的一致性,有助于加合位点的确定。相同的数据表明,在高 pH 条件下,半胱氨酸配对具有足够的灵活性,能够使最初以 S - S 连接的残基与丙烯酰胺络合。同样合理的是,从二维图谱电转印的蛋白质中经常遇到的 -NH(2) 末端封闭可能源于氨甲酰化,而可能与聚丙烯酰胺凝胶中游离的、未反应的丙烯酰胺的烷基化无关。