Abstract: Nuclear magnetic resonance(NMR) technology has evolved into a critical analytical tool for quality research of polysaccharide conjugate vaccines by virtue of its unique advantages of rapid detection, high accuracy and full-spectrum characterization. While current domestic and international guidelines predominantly address small-molecule pharmaceuticals, and there remain gaps in methodological research and regulatory standardization for large-molecules such as polysaccharide-protein conjugates. This article systematically delineates the critical technical distinctions between large- and small-molecule NMR analysis, providing a comparative analysis that spans from inherent molecular structure complexity and instrument parameter requirements to sample preparation rigor and spectral resolution challenges. Combining domestic and international research progress and practical applications, this paper elaborates on the application value of this technology across the full product lifecycle, including process development, the establishment of quality control systems, reference standard characterization and stability studies. On this basis, this paper proposes a review philosophy centered on the concept of “holistic comprehensiveness”. Focusing on issues such as strain identification and the justification of quantitative analysis strategies, it discusses potential new orientations for technical review, so as to offer ideas and references for establishing an NMR analytical standard system for macromolecular biological products.