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Methodology for Structural Analysis of Polysaccharides
Qingbin Guo, Lianzhong Ai, Steve Cui
Verlag Springer-Verlag, 2019
ISBN 9783319963709 , 85 Seiten
Format PDF, OL
Kopierschutz Wasserzeichen
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Contents
6
Abbreviations
9
1 Strategies for Structural Characterization of Polysaccharides
12
1.1 Complexity of Polysaccharide Molecules
12
1.1.1 Monosaccharide Composition
13
1.1.2 Glycosidic Bonds
14
1.1.3 Branching Position and the Degree of Substitution
14
1.1.4 Configurations (?-Form and ?-Form)
15
1.1.5 Special Functional Groups
15
1.1.6 Molecular Weight and Molecular Weight Distribution
16
1.2 Strategies for Structural Characterization of Polysaccharides
16
References
18
2 Polysaccharide Extraction and Fractionation
19
2.1 Extraction and Purification
19
2.2 Fractionation
21
2.2.1 Sequential Ammonium Sulphate Precipitation
21
2.2.2 Sequential Ethanol Precipitation
22
2.2.3 Column Separation
22
2.3 Purity Evaluation of Polysaccharide Samples Prior to Structural Analysis
26
References
26
3 Molecular Weight Distribution and Conformational Properties of Polysaccharides
28
3.1 Triple Detector HPSEC
29
3.1.1 Separation Principle of Size Exclusion Chromatography and Three Calibration Methods of Molecular Weight Determination
29
3.1.2 Conformational Properties of Polysaccharides by HPSEC
29
3.1.3 Branched Structure of Polysaccharides
31
3.2 Batch Mode Multi-angle Light Scattering
33
References
35
4 Monosaccharide Composition Analysis
37
4.1 Complete Hydrolysis
37
4.2 Separations and Detections
38
4.2.1 Anion-Exchange Chromatography
38
4.2.2 GC with Flame Ionization Detection
40
4.2.3 Reverse Phase HPLC Methods
41
4.2.4 Capillary Electrophoresis for Monosaccharide Composition Analysis
42
References
43
5 Partial Acid Hydrolysis and Molecular Degradation
45
5.1 Non-specific Degradation
45
5.1.1 Partial Acid Hydrolysis
45
5.1.2 Ultrasonication Degradation
46
5.2 Controlled Degradation
47
5.2.1 Enzymatic Degradation
47
5.3 Removal of Glycosides from Glycoproteins for Structure Determination
50
References
51
6 Linkage Pattern Analysis
52
6.1 Methylation Analysis
52
6.2 Acidic Polysaccharides Reduction Before Methylation Analysis
54
6.3 Strategies of Methylation Analysis for Glycoprotein or Other Uncommon Sugars
56
6.4 Smith Degradation (Goldstein, Hay, Lewis, & Smith, 1959, 1965)
56
6.4.1 Periodate Oxidation
57
6.4.2 Reduction and Acid Hydrolysis
57
References
58
7 1D & 2D and Solid-State NMR
59
7.1 Sample Preparation
59
7.2 1D NMR
60
7.3 2D NMR
61
7.3.1 COSY Spectrum
62
7.3.2 TOCSY Spectrum
63
7.3.3 HSQC Spectrum
64
7.3.4 Sequence Determination by NOESY and HMBC
65
7.4 Solid-State NMR
67
References
68
8 MALDI-TOF-MS for Polysaccharides Analysis
70
8.1 Introduction
70
8.2 Principles and Procedures (Cui, 2005a)
70
8.3 Applications
71
References
73
9 Fourier Transform Infrared Spectroscopy (FTIR) for Carbohydrate Analysis
74
References
76
10 Detailed Experimental Procedures
77
10.1 Total Sugar Analysis (Phenol-Sulfuric Acid Assay)
77
10.1.1 Sample Preparation
77
10.1.2 Testing Method
77
10.2 Uronic Acid Analysis
78
10.2.1 Sample Preparation
78
10.2.2 Testing Method
78
10.3 Column Separation for Polysaccharides from Flaxseed Hulls
78
10.4 Methylation Analysis
79
10.4.1 Reduction of Uronic Acids
79
10.4.2 Methylation Analysis
80
10.5 Controlled Degradation
81
10.5.1 Periodate Oxidation and Smith Degradation (Ai et al., 2016)
81
10.5.2 Partial Acid Hydrolysis
81
10.5.3 Trifluoromethanesulfonic Acid (TFMS) Hydrolysis
82
10.6 Sample Preparation and Experimental Procedure for NMR Analysis (Guo et al., 2015)
82
References
82
11 Summary
84
Reference
85
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