ANALYTICA CHIMICA ACTA
·
2013
·
IF 4.387
Debin Wan,Hongmei Yang,Fengrui Song,Zhiqiang Liu,Shuying Liu
1-Phenyl-3-methyl-5-pyrazolone (PMP) labeling technique has hitherto proved to be a convenient and sensitive method for separating and detecting oligosaccharides. However, the detailed fragmentation of the derivatives by tandem mass spectrometry has been reported limitedly and no characteristic fragment ions for isomers have been detected. In this study, eight disaccharide isomers were labeled with PMP and analyzed by positive ion electrospray ionization multi-stage tandem mass spectrometry (ESI-MS n ). In comparison with the native disaccharides, PMP labeled disaccharides gave rise to more fragment ions in the tandem mass spectra. The distinctive diagnostic fragment ions formed from cleavage of C C bonds have been detected in the fragmentation of PMP-labeled disaccharide linkage isomers, allowing unambiguous assignment of the position of the glycosidic linkages. This feature is particularly useful for the structural determination of unknown isomeric disaccharides mixed together. In addition, the anomeric configurations can also be easily assigned based on the relative abundance ratios of the selected ion pairs. To verify the feasibility of the method used in the analysis of natural product, water soluble Panax Ginseng extract has been further investigated to identify its unknown disaccharides. The results confirmed that the PMP labeling technique in conjunction with ESI-MS n could offer a powerful and convenient tool for differentiation of structurally closely related isomers, even the unknown mixtures of isomeric disaccharides with different linkage types.
研究领域:
分析化学
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生物化学
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DOI
高影响因子
Scientific Reports
·
2016
·Vol. 6
·期 1
·1-9
·
IF 5.228
Yang Hongmei,Shi Lei,Zhuang Xiaoyu,Su Rui,Wan Debin,Song Fengrui,Li Jinying,Liu Shuying
It remains particularly difficult for gaining unambiguous information on anomer, linkage and position isomers of oligosaccharides using conventional mass spectrometry (MS) methods. In our laboratory, an ion mobility (IM) shift strategy was employed to improve confidence in the identification of structurally closely related disaccharide and monosaccharide isomers using IMMS. Higher separation between structural isomers was achieved using 1-phenyl-3-methyl-5-pyrazolone (PMP) derivatization in comparison with phenylhydrazine (PHN) derivatization. Furthermore, the combination of pre-IM fragmentation of PMP derivatives provided sufficient resolution to separate the isomers not resolved in the IMMS. To chart the structural variation observed in IMMS, the collision cross sections (CCSs) for the corresponding ions were measured. We analyzed nine disaccharide and three monosaccharide isomers that differ in composition, linkages, or configuration. Our data show that coexisting carbohydrate isomers can be identified by the PMP labeling technique in conjunction with ion-mobility separation and tandem mass spectrometry. The practical application of this rapid and effective method that requires only small amounts of sample is demonstrated by the successful analysis of water-soluble ginseng extract. This demonstrated the potential of this method to measure a variety of heterogeneous sample mixtures, which may have an important impact on the field of glycomics.
研究领域:
分析化学
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糖组学
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生物医学
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DOI
高影响因子
Current Research in Food Science
·
2022
·
IF 6.269
Simeng Shao,Weiyin Xu,Zhaoyang Xie,Mengyuan Li,Jingli Zhao,Xinxin Yang,Peng Yu,Hongmei Yang
Despite the widely recognized importance of ginseng carbohydrates, their structural analysis is still challenging due to structural complexity. This study presents the first ion mobility-mass spectrometry (IM-MS) combined with 1-phenyl-3-methyl-5-pyrazolone (PMP) labeling and multivariate data analysis for profiling carbohydrates in the seven ginseng products. 11 carbohydrates were tentatively annotated, including 5 first found in ginseng, and three of them were solely detected in black ginseng (BG) samples, speculated as monosaccharides bearing various groups based on MS 2 analysis. Furthermore, 3D profiles of carbohydrates in IM-MS of the samples showed good discrimination between the varieties of ginseng which were classified into two groups utilizing carbohydrate contents by PLS-DA. The big difference between BG and the others may be ascribed to the repeated heating and steaming process for preparation of BG products. Our findings may provide insights into the differences in bioactivity of different ginseng varieties for future research and show a valuable methodology for discovering unknown carbohydrates.
研究领域:
植物化学
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分析化学
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生物信息学
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产品关联
DOI
PubMed
高影响因子
CARBOHYDRATE RESEARCH
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2015
·
IF 1.929
Zhangrun Han,Yangyang Zeng,Hong Lu,Lijuan Zhang
Chitin is one of the most abundant polysaccharides on earth. It consists of repeating β-1,4 linked N-acetylated glucosamine (A) units. Chitosan is an N-deacetylated product of chitin. Chitosan and its derivatives have broad medical applications as drugs, nutraceuticals , or drug delivery agents. However, a reliable analytical method for quality control of medically used chitosans is still lacking. In current study, nitrous acid was used to cleave all glucosamine residues in chitosan into 2,5-anhydromannose (M) or M at the reducing end of di-, tri-, and oligosaccharides . PMP , i.e. 1-phenyl-3-methyl-5-pyrazolone, was used to label all the Ms. Online UV detection allowed quantification of all M-containing UV peaks whereas online MS analysis directly identified 11 different kinds of mono-, di-, tri-, and oligosaccharides that correlated each oligosaccharide with specific UV peak after HPLC separation. The DA (degree of acetylation) for chitosans was calculated based on the A/(A+M) value derived from the UV data. This newly developed method had several advantages for quality control of chitosan: 1. the experimental procedures were extensively optimized; 2. the reliability of the method was confirmed by online LC-MS analysis; 3. the DA value was obtainable based on the UV data after HPLC analysis, which was comparableto that of 1 H NMR and conductometric titration analyses; 4. finally and most importantly, this method could be used to obtain the DA as well as chemical acetylation/deacetylation mechanisms for chitosan by any laboratory equipped with a HPLC and an online UV detector.
研究领域:
分析化学
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药学
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生物技术
✓ 已验证
产品关联
DOI
PubMed
高影响因子
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