A Practical Guide to the Methylation Analysis of Carbohydrates

A. Retention times of partially methylated alditol acetates

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A Practical Guide

Retention times of partially methylated alditol acetates on gas liquid chromatography using the following phases, ECNSS-M, OV-225, OS-138 and SP-1000.

Gas chromatographys used were Perkin-Elmer models 900 or 990 (for ECNSS-M, OV-225 and OS-138 columns) and a Hewlett Packard model 5830 A (for the SP-1000 column). All were equipped with FID. Oven temperatures are give for each table. Injection and detector temperatures were 25°C higher than the corresponding oven temperatures.
Carrier gas flows were 20-25 mL N2/min for packed columns [180 cm x2.0 mm (I.D)] whilst for the capilary column [25 m x 0.25 mm (I.D.)] a home built splitter (splitting ratio 9:1) was used giving a flow of N2 through the column of 0.4 mL/min. "Make up" gas flow was 30 mL/min.
Abbreviations:
GlyGlycerol
EryErythritol
AraArabinitol
RibRibitol
XylXylitol
GalGalactitol
GlcGlucitol
ManMannitol
FucFucitol
RhaRhamnitol
AbeAbequitol (3,6-dideoxy-D-xylo-hexitol)
ParParatitol (3,6-dideoxy-D-ribo-hexitol)
TyvTyvelitol (3,6-dideoxy-D-arabino-hexitol)
D-Gly-D-GalD-glycero-D-galacto-heptose
D-Gly-D-ManD-glycero-D-manno-heptose
L-Gly-D-ManL-glycero-D-manno-heptose


Relative retention times of partially methylated alditol acetates on an ECNSS-M column (170°C)
location of methyl groupGlyEryAra RibXylGalGlc ManFucRhaAbe ParTyv
20.17- - - 2.928.17.9 7.01.671.52- --
3-0.47- -2.9211.19.6 8.82.051.94- --
4--- -2.9211.111.5 8.82.081.72- --
6--- --5.105.62 4.48--- --
2,3--- -1.545.685.39 4.831.180.98- --
2,4--1.40 -1.346.355.10 5.441.120.990.32 0.340.29
2,5--1.10 --5.80- ---- --
2,6--- --3.653.83 3.35--- --
3,4--1.38 -1.546.935.27 5.37-0.92- --
3,5--0.91 0.771.086.35- 5.44--- --
3,6--- --4.354.40 4.15--- --
4,6--- --3.644.02 3.29--- --
2,3,4--0.73 -0.683.412.49 2.480.650.46- --
2,3,5--0.48 0.40-3.28- -0.62-- --
2,3,6--- --2.422.50 2.20--- --
2,4,6--- --2.281.95 2.09--- --
2,5,6--- --2.25- ---- --
3,4,6--- --2.501.98 1.95--- --
1,3,4,6--- ---0.72 0.72--- --
2,3,4,6--- --1.251.00 1.00--- --
2,3,5,6--- --1.15- ---- --


Relative retention times of partially methylated alditol acetates on an OV-225 column (170°C)
location of methyl groupAraXylGal GlcManFucRha
21.932.15- 6.65.651.431.37
31.482.15- 7.66.8-1.67
4-2.15- 8.46.81.711.57
6--- 5.04.1--
2,31.071.194.7 4.503.69-0.92
2,41.101.065.1 4.214.511.020.94
2,50.84-4.65 ----
2,6--3.14 3.38---
3,4-1.195.5 4.264.36-0.87
3,50.80-5.1 -4.510.96-
3,6--- 3.733.67--
4,6--- 3.492.92--
2,3,40.540.542.89 2.222.190.580.35
2,3,50.41-2.76 --0.47-
2,3,6--2.22 2.322.03--
2,4,6--2.03 1.821.90--
2,5,6--1.95 ----
3,4,6--2.15 1.831.82--
2,3,4,6--1.19 1.000.99--
2,3,5,6--1.10 ----


Relative retention times of partially methylated alditol acetates on an OS-138 column (180°C)
location of methyl groupRibGalGlc ManRha
2--- -1.21
2,3--3.0 -0.86
2,4--- -0.94
2,50.77-- --
3,4--- -0.80
3,50.70-- --
2,3,4-2.521.88 1.930.49
2,3,6-1.741.75 --
2,4,6-1.881.63 --
2,3,4,6-1.161.00 1.00-


Relative retention times of partially methylated alditol acetates on an SP-1000 glass capillary column (220°C)
location of methyl groupXylAraRib GalGlcManFuc Rha
22.04-- -5.064.85- 1.42
32.02-- 6.245.44-- 1.57
4-1.94- -5.95-- 1.48
5--1.29 ---- -
6--- -3.943.41- -
2,31.231.15- 3.663.503.291.02 0.93
2,41.161.23- 4.193.503.801.08 1.00
2,5--- 3.73--- -
2,6--- 2.772.792.65- -
3,4--- 4.143.503.43- 0.88
3,5--0.81 ---- -
3,6--- -2.942.96- -
4,6--- 2.902.922.65- -
2,3,40.67-- 2.422.001.98- 0.48
2,3,5-0.54- 2.38--0.59 -
2,3,6--- 1.861.941.79- -
2,4,6--- 1.941.721.87- -
2,5,6--- ---- -
3,4,6--- 1.961.681.66- -
2,3,4,6--- 1.141.001.00- -
2,3,5,6--- 1.07--- -

Heptose derivatives

Relative retention times of partially methylated alditol acetates on OV-225 (185°)
location of methyl groupD-Gly-D-GalD-Gly-D-ManL-Gly-D-Man
2,4,6--10.6
2,4,77.3--
2,6,7--5.6
2,3,4,6--5.6
2,3,4,74.7--
2,3,6,74.1--
2,4,6,7--4.3
3,4,6,7--4.2
2,3,4,6,72.221.682.3
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