Design of experiments: an efficient strategy to identify factors influencing extraction and derivatization of Arabidopsis thaliana samples in metabolomic studies with gas chromatography/mass spectrometry.

Publisher Summary This chapter describes that mass spectrometry (m.s.) has become an important and versatile technique in carbohydrate chemistry. The chapter deals with m.s. as a tool in the structural analysis of naturally occurring carbohydrates. The mass spectra of permethylated methyl glycosides show ions derived from a number of specific degradation pathways. These fragmentations have been carefully studied in the chapter, by using deuterium-labelling techniques. Direct derivatization of reducing sugars by permethylation, peracetylation, or per( trimethylsilyl )ation gives a mixture of glycosides. These derivatives are suitable for g.1.c. analysis, although, for complex mixtures of sugars, the multiplicity of peaks caused by the derivatization may complicate elucidation of the results. The partially methylated sugars are separated and converted into the methyl glycosides, and these are methylated with trideuteriomethyl iodide. The substitution pattern of the trideuteriomethyl groups can be determined by m.s., and the nature of the sugar ascertained by g.1.c. (by comparison with the permethylated compound used as the reference sample).

Mass Spectrometry in Structural Analysis of Natural Carbohydrates

The determination of carbohydrate in biological materials by gas-liquid chromatography.

Publisher Summary This chapter explains that many developments have taken place in the applications of gas–liquid chromatography to carbohydrates. The chapter discusses a classical paper on the application of trimethylsilyl derivatives of carbohydrates in gas–liquid chromatography. The discovery that these derivatives are readily formed and that they are volatile revolutionized the separation and analysis of carbohydrate mixtures. The chapter reviews the determination of carbohydrates in biological materials by gas–liquid chromatography and the use of this method in the analysis of plant materials. In examining the structure of a polysaccharide, it is convenient to consider the methods involved under the three main headings: (1) quantitative analysis, ( 2 ) methylation, and (3) periodate oxidation. Each of these aspects of polysaccharide chemistry may be aided by the application of gas–liquid chromatography, either qualitative or quantitative, or both. Thus, separations impossible by other techniques may often be achieved, and analytical data obtained in a fraction of the time demanded by other methods.

Applications of Gas-Liquid Chromatography to Carbohydrates :Part I°

Qualitative and quantitative evaluation of mono- and disaccharides in D-fructose, D-glucose and sucrose caramels by gas-liquid chromatography-mass spectrometry. Di-D-fructose dianhydrides as tracers of caramel authenticity.

M. Müller

Papers

Studies on the ring structures of ketoses by means of gas chromatography and mass spectroscopy