CARBOHYDRATE RESEARCH
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2024
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IF 2.4
Xiaofang Ma,Caihong Li,Junyin Zhang,Jiang Xin,Isidore Mosongo,Jiahui Yang,Kaifeng Hu
The physicochemical properties and biological activities of polysaccharides depend on their structures. Monosaccharide composition analysis is indispensable for the structural characterization of polysaccharides and is helpful in the quality control of polysaccharide preparation. Here, using a model mixture and tamarind seed polysaccharide as examples, we demonstrated that a quantitative 2D NMR method, gsHSQC i (three gradient-selective Heteronuclear Single Quantum Coherence spectra acquired with incremented repetition times, i = 1, 2, 3) can directly quantify a variety of monosaccharides in solution with adequate precision and accuracy, requiring no derivatization, postprocessing steps and column separation. Both anomeric and non-anomeric signals of monosaccharides can be utilized for content determination. More accurate quantification of fructose in a mixture containing nine monosaccharides is obtained, which is difficult to achieve by quantitative 1D 1 HNMR and the common PMP-HPLC method (high-performance liquid chromatography through pre-column derivatization with 1-phenyl-3-methyl-5-pyrazolone) due to the peak overlapping and the poor derivatization efficiency, respectively. The results also revealed that Na[Fe(EDTA)] can serve as a proper relaxation-enhancing agent for saccharide samples to save experimental time. We expect that this approach can be applied as an alternative to analyzing the monosaccharide composition and be helpful in interpreting the structure of polysaccharides.
研究领域:
分析化学
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生物化学
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药学
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产品关联
DOI
PubMed
高影响因子
JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS
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2021
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IF 3.935
Yilin Zhang,Mengqi Wu,Jingrui Xi,Chen Pan,Zhizhen Xu,Wei Xia,Wenqing Zhang
In this study, the multiple fingerprints, which were integrated with HPGFC-ELSD (high performance gel filtration chromatography - evaporative light scattering detector) fingerprint, PMP-HPLC-DAD (1-phenyl-3-methyl-5-pyrazolone-high performance liquid chromatography - diode array detector) fingerprint of complete acid hydrolysates and HILIC-HPLC-ELSD (hydrophilic interaction - high performance liquid chromatography - evaporative light scattering detector) fingerprint of enzyme hydrolysates, were established to evaluate the quality of polysaccharides from Poria cocos (PCPs). The similarity evaluation showed that 16 batches of PCPs from different origins had high similarity in structural characteristics based on the multiple fingerprints. The chromatographic data of multiple fingerprints of PCPs were fused, processed and analyzed by chemometric methods including HCA (hierarchical cluster analysis), PCA (principal component analysis) and PLS-DA (partial least squares discriminant analysis). The 16 batches of PCPs were divided into 3 categories in PCA, indicating a certain relationship between the structural characteristics and the origins. PLS-DA analysis indicated that Man, Glc, Gal, Fuc, the components with m/z of 2.22 × 10 4 ∼1.53 × 10 4 Da and 3.46 × 10 3 ∼2.69 × 10 3 Da, oligosaccharides with DPs of 6 and 7, respectively, could be regarded as potential chemical markers for the classification of PCPs from different origins. According to the multiple fingerprints and chemometric analysis, the two commercial samples were proved to be adulterants.
研究领域:
中药学
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分析化学
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产品关联
DOI
PubMed
高影响因子
JOURNAL OF CHROMATOGRAPHY A
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2025
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IF 4
Liang Xu,Jinjian Yao,Zhen Wang,Songzi Xie,Jinmei Ou,Bin Wang
Conventional methods for analyzing monosaccharides, such as 1-Phenyl-3-methyl-5-pyrazolone (PMP) derivatization coupled with high-performance liquid chromatography (HPLC), struggle to detect ketoses and acidic sugars. This limitation hinders the precise structural analysis of polysaccharides in traditional Chinese medicine (TCM). A methylation-assisted Gas Chromatography-Mass Spectrometry (GC–MS) approach was developed to address this issue in the current study. By optimizing the methylation process and using GC–MS with a BR-17 column and an Electron Ionization (EI) source, simultaneous detection of ten different monosaccharides was achieved within 20 min. GC–MS profiling of monosaccharides generally gives two peaks per analyte, except in the cases of fructose and galacturonic acid. Notably, fructose (Fru) was identified for the first time in the polysaccharides of Polygonatum species: P. sibiricum at 18.55 μg/mg, P. cyrtonema at 16.90 μg/mg, and P. kingianum at 14.35 μg/mg, overcoming the limitations of the inability to detect ketoses in the PMP-HPLC method. Data analysis revealed distinct species-specific markers: P. kingianum polysaccharides (PKP) uniquely contained α -galacturonic acid (α-Gal: 19.95 μg/mg), whereas P. sibiricum polysaccharides (PSP) featured six monosaccharides, including glucose (Glc: 135.45 μg/mg), mannose (Man: 78.95 μg/mg), and ribose (Rib: 26.90 μg/mg), with a total of 299.50 μg/mg. P. cyrtonema polysaccharides (PCP) showed elevated levels of glucuronic acid (GlcA, 38.40 μg/mg). This derivatization-enhanced GC–MS method effectively fingerprints TCM polysaccharides, enabling clear differentiation of Polygonatum species through analysis of monosaccharide composition and total sugar content. This approach establishes clear structural distinctions, overcoming the limitations of conventional chromatographic techniques and enhancing the quality control and authentication of TCM polysaccharides.
研究领域:
分析化学
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碳水化合物化学
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植物化学
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中医药学
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质谱分析
✓ 已验证
产品关联
DOI
PubMed
高影响因子
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