含N-非取代葡糖胺残基肝素四糖的制备与表征
生物体内含有N-非取代葡糖胺残基（GlcNH3^＋）结构的硫酸类肝素（HS）具有重要的生物和病理生理学功能。但这种HS在生物体内的含量较少、获得困难,而采用化学方法制备与生物体内结构相似的这种寡糖,有助于研究HS在生物体内的功能作用。本实验以高硫的肝素四糖为原料,用部分脱N位硫酸根的方法,制备了含1个和2个GlcNH3^＋的肝素四糖,并采用液相色谱-离子阱-飞行时间质谱（LC/MS-IT-TOF）法对其进行结构检测。通过分析（EIC）-MS和MS2提取离子流图发现,含不同GlcNH3^＋数目的肝素四糖具有不同的裂解规律,含GlcNH3^＋数目越多,生成的碎片离子越多,这为MS方法进一步鉴定和定...
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| Published in | 质谱学报 Vol. 37; no. 6; pp. 492 - 503 |
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| Main Author | |
| Format | Journal Article |
| Language | Chinese |
| Published |
福州大学糖生物化学研究所,福建 福州,350002
2016
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| Subjects | |
| Online Access | Get full text |
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| Summary: | 生物体内含有N-非取代葡糖胺残基（GlcNH3^＋）结构的硫酸类肝素（HS）具有重要的生物和病理生理学功能。但这种HS在生物体内的含量较少、获得困难,而采用化学方法制备与生物体内结构相似的这种寡糖,有助于研究HS在生物体内的功能作用。本实验以高硫的肝素四糖为原料,用部分脱N位硫酸根的方法,制备了含1个和2个GlcNH3^＋的肝素四糖,并采用液相色谱-离子阱-飞行时间质谱（LC/MS-IT-TOF）法对其进行结构检测。通过分析（EIC）-MS和MS2提取离子流图发现,含不同GlcNH3^＋数目的肝素四糖具有不同的裂解规律,含GlcNH3^＋数目越多,生成的碎片离子越多,这为MS方法进一步鉴定和定量测定含GlcNH3^＋结构的寡糖奠定了基础。 |
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| Bibliography: | hep a rin; tetrasaccharide; N-unsubst ituted disaccharide; liquid chromatog-raphy-ion trap/time-of-flight mass spectrometry （LC /MS- IT-TOF） ; fragmentation pat-tern The rare GlcNH3＋ residues implicated in important cellbiological and patho-physiological phenomena are also now particularly hot subjects in the pharmaceutical industry. Recently its tumour invasion and metastasis has raised interest. However, it is difficult to prepare naturally-occuring, because of their low abundance in GlcNH3 ^＋- containing oligosaccharides from HS. Therefore, the ability to chemically generate a series of structurally-defined oligosaccharides containing GlcNH3＋ residues would greatly contribute to investigating their natural role in HS. In this study, heparin tetrasac- charides （dp4s） possessing one and two GlcNH^＋ residues were prepared from partially de-N-sulfation of the fully sulfated dp4. Then the structure of dp4s was further detected by liquid chromatography-ion trap/time-of-flight mass spectrometry （LC/MS-IT-TOF）. Two |
| ISSN: | 1004-2997 |
| DOI: | 10.7538/zpxb.youxian.2016.0027 |