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TMS (trimethylsilyl) Derivitives of Monosaccharides

Posted: Thu Jun 24, 2010 6:58 pm
by John R. Carver
Does anyone have some GC procedures -including column- for analyzing TMS derivities of monosaccharides.

Posted: Thu Jun 24, 2010 8:13 pm
by chromatographer1
The most commonly used column is 3% OV-17 on Supelcoport (packed column). Injection of 1µL of a 1% hexane solution should be adequate.

Any of the 50% phenyl / 50% methyl silicone phases in commercial capillary columns should be equivalent.

Temperatures of injector ~200°C

Oven temperatures 100-250°C

Use appropriate general use flow rates of carrier gas.

There should be example chromatograms on many chromatography supplies web sites. Do your own Google search.

best wishes,

Rodney George

Posted: Wed Jun 30, 2010 5:27 pm
by Phycal
Use a packed column for this separation as a capillary column will be too resolving. What I mean by this is, TMS is very bulky side group and will add at different places (based on hindrance from other TMS groups) and you would end up with more peaks for each sugar. When I did this on a capillary column using a 30M DB-5 (hydrogen carrier gas), I ended up with 6 peaks per sugar.

Alditol actete with 1-methyl imidazole as the catalyst also is a great derivatization method and you end up with one peak per sugar.