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CARBOHYDRATE RESEARCH · 2024 · IF 2.4

Monosaccharide composition analysis by 2D quantitative gsHSQCi

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.

CAS / MDL: 91510-62-2
研究领域: 分析化学 · 生物化学 · 药学
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JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS · 2021 · IF 3.935

Multiple-fingerprint analysis of Poria cocos polysaccharide by HPLC combined with chemometrics methods

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 · 分析化学
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JOURNAL OF CHROMATOGRAPHY A · 2025 · IF 4

A methylation-assisted gas chromatography-mass spectrometry strategy for comprehensive monosaccharide profiling in Polygonatum polysaccharides: Overcoming limitations of conventional chromatographic techniques

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.

CAS / MDL: 544-76-3
研究领域: 分析化学 · 碳水化合物化学 · 植物化学 · 中医药学 · 质谱分析
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LANGMUIR · 2023 · IF 3.9

The Surface of a PMP Hollow Fiber Membrane Was Modified with a Diamond-like Carbon Film to Enhance the Blood Compatibility of an Artificial Lung Membrane

Donghai Sheng,Lin Zhang,Hongfei Shang,Baoming Guo,Yuan Li

The contact between the blood and the surface of medical materials causes a series of rejection reactions. In this process, the plasma protein is adsorbed to the surface of materials within seconds and binds to glycoprotein receptors on platelets, causing platelet activation, coagulation cascade, and complement activation to form thrombus, which greatly limits the application of medical materials. In our work, the surface of poly(4-methyl-1-pentene) hollow fiber membranes (PMP HFMs) was coated with a diamond-like carbon (DLC) film by the ion plating method. The blood compatibility of the DLC coating was evaluated by protein adsorption, platelet adhesion, clotting time, red blood cell (RBCs) hemolysis, dynamic coagulation, and extracorporeal blood circulation tests. Compared with the unmodified PMP membrane, the DLC film could effectively reduce protein adsorption and platelet adhesion and prolong the coagulation time. The DLC coating showed BSA adsorption of as low as 0.53 μg/cm2 as well as a long activated partial thromboplastin time (APTT) value of 71.84 s. Furthermore, the PMP membrane modified with the DLC coating was used for extracorporeal blood circulation without thrombosis forming within 28 days. The DLC coating is one of the most promising medical coatings as an artificial lung membrane in extracorporeal membrane oxygenation (ECMO) equipment.

研究领域: 生物医学工程 · 材料科学 · 血液学
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JOURNAL OF MEMBRANE SCIENCE · 2025 · IF 9

Engineering fluorinated COF-based hybrid membranes for efficient blood oxygenation

Yuhang Guo,Guangzhaoyao Yang,Shiyao Yu,Jing Huang,Fusheng Pan,Runnan Zhang,Haojun Fan,Zhongyi Jiang

Poly (4-methyl-1-pentene) (PMP) is widely used between blood and gas in extracorporeal membrane oxygenation (ECMO). However, it is more suitable to miniaturize the oxygenator from an economic and biosafety standpoint, that necessitates the PMP oxygenation membrane with enhanced gas permeance and hemocompatibility. This study introduced fluorinated covalent organic framework (FCOF) nanofiber into PMP matrix to construct PMP-FCOF hybrid flat sheet membranes and hollow fiber membranes (HFMs) via thermally induced phase separation (TIPS). FCOF exhibits structural and chemical similarity with PMP, ensuring the good compatibility with PMP matrix. The abundant C–F bonds rendered membrane low-surface-energy of ∼30.2 mN m −1 for PMP–FCOF–3 flat sheet membrane, exhibiting better hemocompatibility compared with that of ∼34.4 mN m −1 for the PMP membrane. The fabricated PMP–FCOF–3 HFMs for blood gas exchange with O 2 exchange rate of ∼309.8 mL min −1 m −2 , which was 77.3 % higher than the commercial PMP HFM, and comparable CO 2 exchange rate of ∼251.7 mL min −1 m −2 with commercial PMP HFM. The blood-gas exchange and hemocompatibility were synergistically enhanced by a simple hybrid strategy, exhibiting great application potentials.

CAS / MDL: 64-19-7 77-90-7 113-38-2
研究领域: 生物医学工程 · 材料科学 · 化学工程
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CARBOHYDRATE POLYMERS · 2024 · IF 10.7

A novel strategy with in vivo characterization, extraction, isolation and activity evaluation for discovery of absorbed anti-inflammatory oligosaccharides from Zhu-Ling decoction

Xi-yang Tang,Zhi-heng Shu,Peng-cheng Zhao,Wen Wei,Cai-lian Fan,Zhi-hong Yao,Xin-sheng Yao,Yi Dai

Zhu-Ling decoction (ZLD), a classical traditional Chinese medicine (TCM) formula, is used for the treatment of chronic kidney diseases. However, the structure and activity of absorbed oligosaccharides (OSs) in ZLD are not clear. In this study, a novel strategy with in vivo characterization, extraction, isolation, activity evaluation was established and applied to identify absorbed anti-inflammatory OSs in ZLD. The results revealed that 30 OSs (22 reducing and 8 non-reducing OSs) and 11 OSs (7 reducing and 4 non-reducing OS) were characterized from ZLD in vitro and in vivo by using UPLC/Q-TOF-MS with PMP derivatization, respectively. Among them, a series of −1 → 3- β -D-Glcp-OSs were isolated and identified by HPLC-HILIC-UVD-ELSD, SPHPLC-HILIC-RID, monosaccharide composition, MS and 1D/2D-NMR spectroscopy, including laminaritriose, laminaritetraose, laminaripentaose, laminarihexaose, laminariheptaose, laminarioctaose and laminarinonaose. Moreover, the 4 non-reducing absorbed OSs were identified by comparison with reference standards, including sucrose, trehalose, raffinose and stachyose. Among them, laminaritriose, laminaritetraose and laminaripentaose significantly inhibited TNF-α and IL-6 levels in LPS-induced HK-2 cell and exerted significant anti-inflammatory effects via the NF-κB and Akt/mTOR signaling pathways. Together, our work provides a novel strategy for discovery of absorbed anti-inflammatory OSs and broadens new horizons for the discovery of in vivo pharmacodynamic substances in TCM formulas.

研究领域: 药理学 · 中药学 · 生物化学 · 分子生物学
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