LC/TOF, LC/HRMS, LC/MS, LC/MS/MS
IndustriesPharma & Biopharma
ManufacturerShimadzu
Significance of the Topic
Peptide mapping is essential for detailed primary structure characterization of monoclonal antibodies (mAbs), enabling detection of single amino acid changes and post-translational modifications (PTMs). A robust, unbiased workflow improves the accuracy and reproducibility of biopharmaceutical quality control.
Study Objectives and Overview
This study demonstrates an integrated data-independent acquisition (DIA) approach on the Shimadzu LCMS-9030 Q-TOF mass spectrometer for de novo peptide sequencing of a bevacizumab biosimilar, aiming to verify the complete primary sequence and identify any structural alterations without relying solely on comparative reference maps.
Methodology and Instrumentation
Sample Preparation:
- Denaturation and reduction: bevacizumab digested in Tris-HCl buffer with ProteaseMAX and DTT.
- Alkylation: iodoacetamide treatment.
- Enzymatic digestion: overnight trypsin incubation.
- Quenching: trifluoroacetic acid addition.
Instrumental Setup:
- Liquid chromatography: Shimadzu Nexera X2 UHPLC with Shim-pack GISS-HP (3 μm, 150 × 3.0 mm) column at 40 °C, gradient from 0% to 75% acetonitrile over 35 min.
- Mass spectrometry: Shimadzu LCMS-9030 Q-TOF with heated electrospray interface, full-scan MS (100–2000 m/z) and MS/MS DIA segments covering 210–1690 m/z in 40 m/z windows.
- Data processing: MS-DIAL for peak extraction, Skyline for theoretical y and b ion transition prediction.
Results and Discussion
The workflow extracted 11 852 mass features, leading to confident identification of 61 tryptic peptides (42 heavy-chain and 19 light-chain) covering 100% of the mAb sequence. The example peptide ALPAPIEK exhibited clear matching of extracted MS/MS fragments to predicted transitions, validating the de novo sequencing capability. Observations included PTMs such as N-glycosylation and C-terminal lysine processing.
Benefits and Practical Applications
- Unbiased fragmentation: DIA captures all fragment ions without precursor selection, enhancing sequence coverage.
- Comprehensive mapping: full amino acid coverage and detection of PTMs supports in-depth characterization.
- Improved reproducibility: standardized UHPLC-Q-TOF conditions reduce variability in comparative analyses.
- Regulatory compliance: robust primary structure confirmation aligns with biopharma quality requirements.
Future Trends and Opportunities
Advancements may include machine learning-driven spectral interpretation for automated de novo sequencing, integration of real-time PTM monitoring, expansion of DIA methods to other large biomolecules, and streamlined QC workflows incorporating high-throughput peptide mapping.
Conclusion
The described DIA strategy on the LCMS-9030 Q-TOF provides a straightforward, high-coverage approach for de novo peptide sequencing of mAbs, offering significant benefits for biopharmaceutical characterization and quality control.
References
- Searle BC, Pino LK (2018) Chromatogram libraries improve peptide detection and quantification by data independent acquisition mass spectrometry. Nat Commun 9:5128.
- Riken MS-DIAL software for metabolomics and DIA processing.
- MacLean B et al. Skyline: an open source document editor for targeted proteomics.
- Shimadzu (2019) Peptide mapping of monoclonal antibody using LCMS-9030 Q-TOF. Application News AD-0212B.
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