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学者姓名：梁群焘
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Abstract ：
为了进一步探讨非还原端饱和结构的肝素寡糖在UV 232 nm的吸收情况,制备了4种饱和结构的肝素二糖,并用离子对反相液相色谱/离子阱飞行时间质谱(RPIP-LC/MS-IT-TOF)光电二极管阵列检测器分析了它们在UV 232 nm的吸收情况.分析结果表明,饱和结构的肝素二糖在UV 232 nm的检出限为9μg(S/N=10),UV232 nm/UV 206 nm约为不饱和结构肝素二糖UV 232 nm的7%～40%.结果还表明,肝素二糖UV 232 nm的吸收强度受亚硫酸基团(SO_3~(2-))影响较大.另外,通过比较不饱和结构的肝素/硫酸类肝素(Hep/HS)标样二糖发现,含N-未取代葡...
Keyword ：
测序 测序 紫外吸收 紫外吸收 肝素 肝素 质谱 质谱 饱和结构 饱和结构
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| GB/T 7714 | 梁群焘 , 邹强 , 林江慧 et al. 肝素非还原端饱和结构的紫外吸收研究及在肝素寡糖测序中的应用 [J]. | 高等学校化学学报 , 2021 , 42 (06) : 1776-1784 . |
| MLA | 梁群焘 et al. "肝素非还原端饱和结构的紫外吸收研究及在肝素寡糖测序中的应用" . | 高等学校化学学报 42 . 06 (2021) : 1776-1784 . |
| APA | 梁群焘 , 邹强 , 林江慧 , 刘树滔 , 魏峥 . 肝素非还原端饱和结构的紫外吸收研究及在肝素寡糖测序中的应用 . | 高等学校化学学报 , 2021 , 42 (06) , 1776-1784 . |
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Abstract ：
肝素/硫酸乙酰肝素(Hep/HS)寡糖结构多样,且与生物学、病理学功能息息相关,表征这些结构对解析它们的功能具有重要意义。本实验以市售猪肠肝素钠为原料,制备了9种肝素四糖,并用二糖组分分析方法结合反相离子对试剂色谱-串联离子阱飞行时间质谱(IPRP-LC/IT-TOF MS)进行结构解析。结果表明:9种肝素四糖中有两组同分异构体,且含己胺离子对试剂的RP-LC/MS能够成功分离肝素寡糖及其同分异构体;采用LC-MS/MS方法可以鉴定其中一组同分异构体的结构。该方法可为HS/Hep寡糖的研究提供标准品,并为解析HS/Hep同分异构体结构提供一种简单有效的方法,进而为更好地理解生物体内HS/Hep...
Keyword ：
同分异构体 同分异构体 四糖 四糖 液相色谱-串联质谱(LC-MS/MS) 液相色谱-串联质谱(LC-MS/MS) 肝素/硫酸类肝素 肝素/硫酸类肝素
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| GB/T 7714 | 杜佳燕 , 苏晓明 , 梁群焘 et al. 肝素/硫酸乙酰肝素四糖同分异构体的制备与表征 [J]. | 质谱学报 , 2020 , 41 (01) : 28-38 . |
| MLA | 杜佳燕 et al. "肝素/硫酸乙酰肝素四糖同分异构体的制备与表征" . | 质谱学报 41 . 01 (2020) : 28-38 . |
| APA | 杜佳燕 , 苏晓明 , 梁群焘 , 邹强 , 魏峥 . 肝素/硫酸乙酰肝素四糖同分异构体的制备与表征 . | 质谱学报 , 2020 , 41 (01) , 28-38 . |
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Abstract ：
Heparin (Hep) and heparan sulfate (HS) are complex, sulfated GAGs consist of repeating disaccharide units each composed of a uronic acid, either glucuronate or iduronate [the latter sometimes sulfated at C-2, i.e. IdoA2S], and a derivative of glucosamine [either N-acetylglucosamine, N-sulfated glucosamine, or unsubstituted glucosamine] that can be variably O-sulfated. Hep/HS has important biological functions in developmental processes, angiogenesis, blood coagulation, cell adhesion, and tumour metastasis. These involve interactions with a wide variety of proteins, i.e. enzymes, cytokines, growth factors and extracellular matrix proteins through their specific sequences, patterns or densities of sulfation. Mass spectroscopy is now becoming a much more useful tool for the structural analysis of Hep/HS oligosaccharides because of its high detection sensitivity and molecular specificity. MS/MS of heparin/HS oligosaccharides can produce information-rich glycosidic and cross-ring product ions which can be used to determine the sites of acetylation or sulfation. In particular, LC-MS clearly has the potential now to sequence most oligosaccharides, especially with the recent development of a computational framework for dealing with the complex data generated. In this study, porcine intestines heparin was digested by heparinase I. The obtained crude tetrasaccharides (dp4s) were separated and further purified by strong anion-exchange HPLC and size-exclusion HPLC. The structures of dp4s were then investigated by the combination of disaccharide analysis, reversed-phase liquid chromatography/electrospray ionization ion trap/time-of-flight mass spectrometry (RP-LC/ESI-IT/TOF MS) and a computational simulation method. The results showed that nine tetrasaccharides (dp4s) were obtained, in which two series of dp4s isomer were existed. The dp4 isomers were successfully separated using IPRP-LC/MS system with hexylamine. One series of dp4s contains HexA(2S)-GlcNS and HexA(2S)-GlcNS(6S) disaccharides, and other ones possess HexA-GlcNS(6S) and HexA(2S)-GlcNS(6S). Because MSn analysis could produce abundant structurally useful fragments, the former dp4 isomers were selected to investigate fragmentation patterns for the further potential structure analysis by MS. MS2 analysis indicated that one dp4 was HexA(2S)-GlcNS- HexA(2S)-GlcNS(6S) which had one glycosidic cleavage Y1, two cross-ring cleavages 0,2A2 and 0,3A2 in the first glucosamine residues (from the non-reducing end) of oligosaccharide. In contrast, the other dp4 was HexA(2S)-GlcNS(6S)-HexA(2S)-GlcNS which contained two glycosidic cleavages B2 and Y1, two cross-ring cleavages 1,4A2 and 0,3A2 in the first glucosamine residues, and a cross-ring cleavages 1,5X4 in the first glucuronic acid residues of the oligosaccharide. This study provides a simple and efficient method for identifying the sequences of the Hep/HS oligosaccharide isomers, which might lead to a greater understanding of the biological roles of Hep/HS oligosaccharides in organisms. © 2020, Editorial Board of Journal of Chinese Mass Spectrometry Society. All right reserved.
Keyword ：
Acetylation Acetylation Cell adhesion Cell adhesion Drug products Drug products Glucosamine Glucosamine Glucose Glucose Hydraulic structures Hydraulic structures Ionization of liquids Ionization of liquids Ions Ions Isomers Isomers Liquid chromatography Liquid chromatography Mass spectrometry Mass spectrometry Oligosaccharides Oligosaccharides Plants (botany) Plants (botany) Polysaccharides Polysaccharides Proteins Proteins Sulfur compounds Sulfur compounds
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| GB/T 7714 | Du, Jia-Yan , Su, Xiao-Ming , Liang, Qun-Tao et al. Preparation and Characterization of Heparin/Heparan Sulfate Tetrasaccharide Isomers [J]. | Journal of Chinese Mass Spectrometry Society , 2020 , 41 (1) : 28-38 . |
| MLA | Du, Jia-Yan et al. "Preparation and Characterization of Heparin/Heparan Sulfate Tetrasaccharide Isomers" . | Journal of Chinese Mass Spectrometry Society 41 . 1 (2020) : 28-38 . |
| APA | Du, Jia-Yan , Su, Xiao-Ming , Liang, Qun-Tao , Zou, Qiang , Wei, Zheng . Preparation and Characterization of Heparin/Heparan Sulfate Tetrasaccharide Isomers . | Journal of Chinese Mass Spectrometry Society , 2020 , 41 (1) , 28-38 . |
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Colla corii asini (CCA) made from donkey-hide has been widely used as a health-care food and an ingredient of traditional Chinese medicine. Heparan sulfate (HS)/heparin is a structurally complex class of glycosaminoglycans (GAGs) that have been implicated in a wide range of biological activities. However, their presence within CCA, and their possible structural characteristics, were previously unknown. In this study, GAG fractions containing HS/heparin were isolated from CCA and their disaccharide compositions were analyzed by high sensitivity liquid chromatography-ion trap/time-of-flight mass spectrometry (LC-MS-ITTOF). This revealed that, in addition to the eight commonly seen HS disaccharides, the four rare N-unsubstituted disaccharides were also detected in significant quantities. The disaccharide compositions varied significantly between HS/heparin fractions indicating chains with differing domain structures. This novel structural information may lead to a better understanding of the biological activities (i.e. anticoagulation and antitumor action) of CCA. © 2019, Springer Science+Business Media, LLC, part of Springer Nature.
Keyword ：
Colla corii asini; Heparan sulfate; Heparin; LC-MS-ITTOF; N-unsubstituted disaccharide Colla corii asini; Heparan sulfate; Heparin; LC-MS-ITTOF; N-unsubstituted disaccharide
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| GB/T 7714 | Du, J. , Liu, S. , Liang, Q. et al. Analysis of Heparan sulfate/heparin from Colla corii asini by liquid chromatography-electrospray ion trap mass spectrometry [J]. | Glycoconjugate Journal , 2019 , 36 (3) : 211-218 . |
| MLA | Du, J. et al. "Analysis of Heparan sulfate/heparin from Colla corii asini by liquid chromatography-electrospray ion trap mass spectrometry" . | Glycoconjugate Journal 36 . 3 (2019) : 211-218 . |
| APA | Du, J. , Liu, S. , Liang, Q. , Lin, J. , Jiang, L. , Chen, F. et al. Analysis of Heparan sulfate/heparin from Colla corii asini by liquid chromatography-electrospray ion trap mass spectrometry . | Glycoconjugate Journal , 2019 , 36 (3) , 211-218 . |
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本发明提供一种从蛤蟆油中提取硫酸软骨素/硫酸皮肤素/透明质酸的方法。所述方法先将蛤蟆油充分溶胀后加入的胰蛋白酶酶解蛤蟆油，再通过DEAE阴离子交换色谱柱提取蛤蟆油中的糖胺聚糖OR‑GAG，然后经透析、冻干、浓缩后，用硫酸软骨素ABC酶特异性酶解OR‑GAG，足量的酶可将长链酶解至硫酸软骨素/硫酸皮肤素/透明质酸(CS/DS/HA)二糖单元。CS/DS/HA二糖单元经2‑氨基吖啶酮荧光标记后，利用LC/MS‑ITTOF进行结构分析，得到蛤蟆油中各二糖组分的结构与摩尔百分比。
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| GB/T 7714 | 魏峥 , 黄海月 , 林江慧 et al. 一种从蛤蟆油中提取硫酸软骨素/硫酸皮肤素/透明质酸的方法 : CN201910995448.4[P]. | 2019/10/18 . |
| MLA | 魏峥 et al. "一种从蛤蟆油中提取硫酸软骨素/硫酸皮肤素/透明质酸的方法" : CN201910995448.4. | 2019/10/18 . |
| APA | 魏峥 , 黄海月 , 林江慧 , 梁群焘 . 一种从蛤蟆油中提取硫酸软骨素/硫酸皮肤素/透明质酸的方法 : CN201910995448.4. | 2019/10/18 . |
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生物体内含有N-非取代葡糖胺残基(GlcNH_3~+)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GlcNH_3~+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GlcNH_3~+数目的肝素四糖具有不同的裂解规律,含GlcNH_3~+数目越多,生成的碎片离子越多,这为MS方法进一步...
Keyword ：
N-非取代葡糖胺二糖 N-非取代葡糖胺二糖 四糖 四糖 液相色谱-离子阱-飞行时间质谱(LC/MS-IT-TOF) 液相色谱-离子阱-飞行时间质谱(LC/MS-IT-TOF) 肝素 肝素 裂解规律 裂解规律
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| GB/T 7714 | 梁群焘 , 魏峥 . 含N-非取代葡糖胺残基肝素四糖的制备与表征 [J]. | 质谱学报 , 2016 , 37 (06) : 492-503 . |
| MLA | 梁群焘 et al. "含N-非取代葡糖胺残基肝素四糖的制备与表征" . | 质谱学报 37 . 06 (2016) : 492-503 . |
| APA | 梁群焘 , 魏峥 . 含N-非取代葡糖胺残基肝素四糖的制备与表征 . | 质谱学报 , 2016 , 37 (06) , 492-503 . |
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The rare N-unsubstituted glucosamine (GlcNH(3)(+)) residues in heparan sulfate (HS) have important biological and pathophysiological roles. In this study, a high-resolution method for the separation and analysis of N-unsubstituted disaccharides of heparin/HS is described. Four N-unsubstituted disaccharides, together with eight N-substituted species, can be well-separated by ion-pair reverse-phase ultra-performance liquid chromatography. Each disaccharide can then be detected and its relative abundance quantified using electrospray ionization mass spectrometry in the negative mode. Because of its high sensitivity, without interference from proteins and other sample impurities, this method is particularly useful in the analysis of low content GlcNH(3)(+) residues in small amounts of biological materials, eg. sera, tissue and cell culture-derived samples. This would lead to a better understanding of the biological origin of GlcNH(3)(+) residues and their increasingly important function in human health and disease. (C) 2016 Elsevier B.V. All rights reserved.
Keyword ：
Heparan sulfate Heparan sulfate Heparin Heparin LC-MS-ITTOF LC-MS-ITTOF N-unsubstituted disaccharide N-unsubstituted disaccharide
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| GB/T 7714 | Du, Jia Yan , Chen, Lan Rong , Liu, Su et al. Ion-pairing liquid chromatography with on-line electrospray ion trap mass spectrometry for the structural analysis of N-unsubstituted heparin/heparan sulfate [J]. | JOURNAL OF CHROMATOGRAPHY B-ANALYTICAL TECHNOLOGIES IN THE BIOMEDICAL AND LIFE SCIENCES , 2016 , 1028 : 71-76 . |
| MLA | Du, Jia Yan et al. "Ion-pairing liquid chromatography with on-line electrospray ion trap mass spectrometry for the structural analysis of N-unsubstituted heparin/heparan sulfate" . | JOURNAL OF CHROMATOGRAPHY B-ANALYTICAL TECHNOLOGIES IN THE BIOMEDICAL AND LIFE SCIENCES 1028 (2016) : 71-76 . |
| APA | Du, Jia Yan , Chen, Lan Rong , Liu, Su , Lin, Jiang Hui , Liang, Qun Tao , Lyon, Malcolm et al. Ion-pairing liquid chromatography with on-line electrospray ion trap mass spectrometry for the structural analysis of N-unsubstituted heparin/heparan sulfate . | JOURNAL OF CHROMATOGRAPHY B-ANALYTICAL TECHNOLOGIES IN THE BIOMEDICAL AND LIFE SCIENCES , 2016 , 1028 , 71-76 . |
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The rare GlcNH3+ residues implicated in important cellbiological and pathophysiological 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 tetrasaccharides (dp4s) possessing one and two GlcNH3+ 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 dp4s (dp4-1 and dp4-2) are obtained, in which dp4-1 with one GlcNH3+ residue located in the central position, while dp4-2 with two GlcNH3+ residues located in the central and reducing terminal positions. The results of extracted ion chromatogram (EIC) in LC/MS-IT-TOF system suggest that minor sulfate losses of the dp4s appear in MS ion source, but most of the samples maintain the original structure, which is helpful for determining the accurate molecular weight of heparin/HS oligosaccharides with GlcNH3+ residues. MS and MS2 analysis show different fragmentation patterns of dp4s with different GlcNH3+ residues using the same MS parameters. 0,2X2 fragmentation near the non-reducing end of oligosaccharide was only detected in dp4-1. Meanwhile, 1,5X2, 2,4A4 and 1,5A4 fragmentations were only appeared in dp4-2. The dp4 with higher GlcNH3+ residues revealed more cross-ring cleavage patterns, suggesting that higher positive charges might make the ring more fragile, presumably reflecting the markedly different conformations and chemical environments at these positions, which results in different dissociation of dp4s in MS. This provides a foundation for further structural identification and quantification of GlcNH3+-oligosaccharides by mass spectrum analysis, which could lead to a greater understanding of the biological roles of GlcNH3+ residues in HS/heparin. © 2016, Editorial Board of Journal of Chinese Mass Spectrometry Society. All right reserved.
Keyword ：
Chromatographic analysis Chromatographic analysis Drug products Drug products Hydraulic structures Hydraulic structures Ion chromatography Ion chromatography Ion sources Ion sources Mass spectrometry Mass spectrometry Oligosaccharides Oligosaccharides Polysaccharides Polysaccharides Spectrum analysis Spectrum analysis Sulfur compounds Sulfur compounds
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| GB/T 7714 | Liang, Qun-Tao , Wei, Zheng . Preparation and characterization of heparin tetrasaccharide with N-unsubstituted glucosamine residues [J]. | Journal of Chinese Mass Spectrometry Society , 2016 , 37 (6) : 492-503 . |
| MLA | Liang, Qun-Tao et al. "Preparation and characterization of heparin tetrasaccharide with N-unsubstituted glucosamine residues" . | Journal of Chinese Mass Spectrometry Society 37 . 6 (2016) : 492-503 . |
| APA | Liang, Qun-Tao , Wei, Zheng . Preparation and characterization of heparin tetrasaccharide with N-unsubstituted glucosamine residues . | Journal of Chinese Mass Spectrometry Society , 2016 , 37 (6) , 492-503 . |
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The rare N-unsubstituted glucosamine (GlcNH(3) (+)) residues in heparan sulfate (HS) have important biological and pathophysiological roles. Therefore, the ability to chemically generate a series of oligosaccharides, which have a similar structure to the naturally-occurring, GlcNH(3) (+) - containing oligosaccharides from HS, would greatly contribute to investigating their natural role in HS. In this study, a hexasaccharide library that possess GlcNH(3) (+) residues were prepared from the chemical modification of the fully sulfated dp6. Chemical reaction conditions were optimized to generate different pattern of GlcNH(3) (+) - containing oligosaccharides, then the structure of the library was detected by high-performance liquid chromatography-ion trap/time-of-flight mass spectrometry (LC/MS-ITTOF) analysis. EIC/MS and MS2 analysis showed different fragmentation patterns of dp6s with different GlcNH(3) (+) residues. This provides a foundation for further identification and quantification of GlcNH(3) (+) - oligosaccharides by mass spectrum analysis.
Keyword ：
Heparin Heparin Hexasaccharide Hexasaccharide LC-MS-ITTOF LC-MS-ITTOF N-unsubstituted disaccharide N-unsubstituted disaccharide
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| GB/T 7714 | Liang, Qun Tao , Du, Jia Yan , Fu, Qing et al. Preparation and characterization of heparin hexasaccharide library with N-unsubstituted glucosamine residues [J]. | GLYCOCONJUGATE JOURNAL , 2015 , 32 (8) : 643-653 . |
| MLA | Liang, Qun Tao et al. "Preparation and characterization of heparin hexasaccharide library with N-unsubstituted glucosamine residues" . | GLYCOCONJUGATE JOURNAL 32 . 8 (2015) : 643-653 . |
| APA | Liang, Qun Tao , Du, Jia Yan , Fu, Qing , Lin, Jiang Hui , Wei, Zheng . Preparation and characterization of heparin hexasaccharide library with N-unsubstituted glucosamine residues . | GLYCOCONJUGATE JOURNAL , 2015 , 32 (8) , 643-653 . |
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本发明涉及一种含N-非取代葡萄糖胺(GlcNH3+)肝素六糖的制备及其纯化。所述方法是以酶解低分子量肝素为原料，通过凝胶色谱和离子交换高效液相色谱等方法分离提纯肝素钠六糖；利用阳离子交换树脂和吡啶中和法制备肝素吡啶六糖；最后用脱N-硫酸化法制备含不同GlcNH3+数目的肝素六糖，并用SAX-HPLC等方法进行分离提纯。本方法可特异性制备出含不同GlcNH3+数目和序列的系列肝素寡糖，为硫酸类肝素中GlcNH3+残基的结构与功能及其与疾病关系的研究提供重要的糖库。
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| GB/T 7714 | 魏峥 , 梁群焘 , 林江慧 et al. 含N-非取代葡萄糖胺肝素六糖的制备及其纯化 : CN201410019945.8[P]. | 2014/1/17 . |
| MLA | 魏峥 et al. "含N-非取代葡萄糖胺肝素六糖的制备及其纯化" : CN201410019945.8. | 2014/1/17 . |
| APA | 魏峥 , 梁群焘 , 林江慧 , 魏可镁 . 含N-非取代葡萄糖胺肝素六糖的制备及其纯化 : CN201410019945.8. | 2014/1/17 . |
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