Jiangsu Collaborative Innovation Center of Biomedical Functional Materials, Jiangsu Key Laboratory of Biomedical Materials, School of Chemistry and Materials Science, Nanjing Normal University, Nanjing, China.
Department of Chemistry, University of British Columbia, Vancouver, BC, Canada.
Rapid Commun Mass Spectrom. 2021 Aug 30;35(16):e9139. doi: 10.1002/rcm.9139.
Herbal polysaccharides have various potential medicinal values. Development of reliable analytical method for the fingerprint analysis of polysaccharides is critical for their quality assessment, origin identification, and authenticity evaluation.
Mechanochemical extraction (MCE) was used to extract polysaccharide components from different herbal species. Intact polysaccharides were then directly analyzed by direct analysis in real-time mass spectrometry (DART-MS). Standard addition method with isotope-labeled internal standard was used to quantify polysaccharide amounts directly from liquid extract. Multivariate data analysis was further conducted for species classification.
The intact and large polysaccharides were decomposed into small fragment ions less than m/z 350 instantaneously using DART ion source. Different polysaccharides showed distinguished fingerprint DART-MS spectra using both individual and mixed herbal species. The liquid supernatant from MCE was validated to be used as direct sample for DART-MS analysis. Quantitation was successfully achieved for polysaccharide contents in Dendrobium officinale from different locations.
A rapid fingerprint protocol in combination of MCE and DART-MS for herbal polysaccharides was developed. The whole process could be accomplished within a few minutes, from raw materials to final spectra, without requirements of pre-digestion and additional sample purification.
草药多糖具有多种潜在的药用价值。开发可靠的多糖指纹分析方法对于其质量评估、来源鉴定和真实性评估至关重要。
机械化学提取（MCE）用于从不同草药物种中提取多糖成分。然后直接通过实时直接分析质谱（DART-MS）分析完整的多糖。使用同位素标记内标标准添加法直接从液体提取物中定量多糖含量。进一步进行多元数据分析以进行物种分类。
使用 DART 离子源，完整的大型多糖瞬间分解成小于 m/z 350 的小碎片离子。使用单个和混合草药物种，不同的多糖显示出不同的指纹 DART-MS 光谱。MCE 的上清液被验证可作为 DART-MS 分析的直接样品。成功实现了来自不同产地的铁皮石斛多糖含量的定量。
开发了一种结合 MCE 和 DART-MS 的草药多糖快速指纹图谱方案。整个过程可以在几分钟内完成，从原材料到最终图谱，无需预先消化和额外的样品纯化。
