Department of Chemistry , University of Virginia , Charlottesville , Virginia 22904 , United States.
Department of Pathology , University of Virginia , Charlottesville , Virginia 22908 , United States.
Anal Chem. 2019 Nov 5;91(21):13547-13554. doi: 10.1021/acs.analchem.9b02666. Epub 2019 Oct 16.
Accurate sequence characterization is essential for the development of therapeutic antibodies by the pharmaceutical industry. Presented here is a methodology to obtain comprehensive sequence analysis of a monoclonal antibody. An enzyme reactor of immobilized Aspergillopepsin I, a highly stable nonspecific protease, was used to cleave reduced antibody subunits into a peptide profile ranging from 1 to 20 kDa. Utilizing the Thermo Orbitrap Fusion's unique instrument architecture combined with state-of-the-art instrument control software allowed for dynamic instrument methods that optimally characterize eluting peptides based on their size and charge density. Using a data-dependent instrument method, both collisional dissociation and electron transfer dissociation were used to fragment the appropriate charge state of analyte peptides. The instrument layout also allowed for scans to be taken in parallel using both the ion trap and Orbitrap concurrently, thus allowing larger peptides to be analyzed in high resolution using the Orbitrap while simultaneously analyzing tryptic-like peptides using the ion trap. We harnessed these capabilities to develop a custom method to optimally fragment the eluting peptides based on their mass and charge density. Using this approach, we obtained 100% sequence coverage of the total antibody in a single chromatographic analysis, enabling unambiguous sequence assignment of all residues.
准确的序列特征对于制药行业开发治疗性抗体至关重要。本文介绍了一种获得单克隆抗体全面序列分析的方法。使用固定化 Aspergillopepsin I 酶反应器,一种高度稳定的非特异性蛋白酶,将还原的抗体亚基切割成肽谱,范围从 1 到 20 kDa。利用 Thermo Orbitrap Fusion 独特的仪器架构和最先进的仪器控制软件,允许使用动态仪器方法,根据洗脱肽的大小和电荷密度最佳地对其进行特征描述。使用数据依赖的仪器方法,同时使用碰撞解离和电子转移解离来碎裂分析物肽的适当电荷状态。仪器布局还允许同时使用离子阱和 Orbitrap 并行进行扫描,从而允许使用 Orbitrap 分析较大的肽,同时使用离子阱分析胰蛋白酶样肽。我们利用这些功能开发了一种定制方法,根据洗脱肽的质量和电荷密度来最佳地碎裂它们。使用这种方法,我们在单次色谱分析中获得了总抗体的 100%序列覆盖率,从而能够对所有残基进行明确的序列分配。