Medicinal Plants Classification Biosynthesis and ... - Index of

Quality Control of Polysaccharides from Medicinal Plants and Fungi
Table 4. The methods for analysis of glycosidic linkage in polysaccharides
Techniques Methods
Sample preparation Column Detection
GC
HPLC
IR
NMR
Hydrolysis:
TFA, H 2SO 4, MeOH–
HCl or Formic acid
Derivatization:
partially methylated
aditol acetates
Treated by galactanase
and RG-hydrolase
Powdered samples
were dispersed in KBr
pellets
BPX-series, CP-Sil 5
CP, DB-series, HPseries,
OV-series, SPB-
1, Supelco SP series
column or 3% ECNSS-
M and 1% OV-225
paked column
FID or
MS
TSKgel series MALDI-
TOF MS
Ref.
291
24, 25, 28, 34, 36, 40-
43, 45, 46, 48-51, 53-
60, 62, 63, 65, 83, 100,
119, 120, 122, 131,
136, 158, 185, 162,
165, 167, 174, 176,
178-180, 182-184,
186-189, 212
194
- - 213
D 2O solution - - 20-22, 40, 41, 47-52,
54, 56-59, 104, 120-
122, 141, 165, 174,
176, 183, 204
DMSO-δ6 solution - - 179
GC, Gas chromatography; HPLC, High performance liquid chromatography; IR, Infrared
spectroscopy; NMR, Nuclear magnetic resonance; FID, Flame ionisation detector; MS, Mass
spectrometery; TFA, Trifluoroacetic acid; D 2O, Heavy water; DMSO, Dimethylsulfoxide;
MALDI-TOF MS, Matrix-assisted laser desorption/ionization-time of flight mass spectrometery.
Several NMR spectroscopic methods have been developed that permit the determination
of linkage positions in oligosaccharides [202,203]. The altered chemical shift (δ) also
indicated the configuration of glycosidic linkages, and their ratio could be calculated based
on their relative peak area. NMR with [204-206] or without [203] assistance of other methods
has been applied for elucidation of anomeric configurations. In addition, MS has become one
of the most powerful and versatile techniques for structural analysis of carbohydrates [207-
209]. The most widely used mass spectrometric approach is electrospray ionization (ESI)
tandem-MS, typically performed on triple-quadrupole instruments using precursor-ion
selection in a first MS step, collision-induced dissociation and mass analysis of fragment ions
in a second MS step [210]. However, ESI are not widely used for direct analysis of neutral
glycans due to the ionization is poor. Thus, the derivatization is usually applied prior to ESI-
MS characterization with the aim of increasing analytical performance and sensitivity [211].