Department of Biosciences, Bioanalytical Research Labs, University of Salzburg, Hellbrunner Straße 34, 5020, Salzburg, Austria.
Christian Doppler Laboratory for Innovative Tools for Biosimilar Characterization, University of Salzburg, Hellbrunner Straße 34, 5020, Salzburg, Austria.
Sci Rep. 2020 Oct 22;10(1):18080. doi: 10.1038/s41598-020-75045-1.
In recent years, advanced HPLC-MS strategies based on intact protein ("top-down") or protein subunit ("middle-up/middle-down") analysis have been implemented for the characterization of therapeutic monoclonal antibodies. Here, we assess feasibility of middle-up/middle-down analysis for polyclonal IgGs exhibiting extensive sequence variability. Specifically, we addressed IgGs from mouse, representing an important model system in immunological investigations. To obtain Fc/2 portions as conserved subunits of IgGs, we made use of the bacterial protease SpeB. For this purpose, we initially determined SpeB cleavage sites in murine IgGs. The resulting Fc/2 portions characteristic of different subclasses were subsequently analysed by ion-pair reversed-phase HPLC hyphenated to high-resolution mass spectrometry. This enabled simultaneous relative quantification of IgG subclasses and their N-glycosylation variants, both of which influence IgG effector functions. To assess method capabilities in an immunological context, we applied the analytical workflow to polyclonal antibodies obtained from BALB/c mice immunized with the grass pollen allergen Phl p 6. The study revealed a shift in IgG subclasses and Fc-glycosylation patterns in total and antigen-specific IgGs from different mouse cohorts, respectively. Eventually, Fc/2 characterization may reveal other protein modifications including oxidation, amino acid exchanges, and C-terminal lysine, and may thus be implemented for quality control of functional antibodies.
近年来,基于完整蛋白质(“自上而下”)或蛋白质亚基(“中-上/中-下”)分析的先进 HPLC-MS 策略已被用于治疗性单克隆抗体的表征。在这里,我们评估了广泛存在序列变异的多克隆 IgGs 进行中-上/中-下分析的可行性。具体而言,我们研究了来自小鼠的 IgGs,这是免疫研究中的重要模型系统。为了获得作为 IgGs 保守亚基的 Fc/2 部分,我们利用了细菌蛋白酶 SpeB。为此,我们首先确定了小鼠 IgGs 中的 SpeB 切割位点。随后,使用离子对反相 HPLC 与高分辨率质谱联用分析了具有不同亚类特征的 Fc/2 部分。这使得 IgG 亚类及其 N-糖基化变体的同时相对定量成为可能,而这些变体都影响 IgG 的效应功能。为了在免疫学背景下评估方法的能力,我们将分析工作流程应用于用草花粉过敏原 Phl p 6 免疫的 BALB/c 小鼠获得的多克隆抗体。该研究分别揭示了不同小鼠群体中总 IgG 和抗原特异性 IgG 中 IgG 亚类和 Fc-糖基化模式的变化。最终,Fc/2 表征可能揭示其他蛋白质修饰,包括氧化、氨基酸交换和 C 末端赖氨酸,因此可用于功能性抗体的质量控制。