Development and validation of a GC-MS method for quantification of glycolaldehyde formed from carbohydrate fragmentation processes.

Glycolaldehyde is a small sugar-like molecule that is readily formed by thermochemical fragmentation of carbohydrates and has similar physico-chemical properties as sugars. Current methods for analysis of glycolaldehyde comprise of low selective and time-consuming chromatographic or spectroscopic techniques such as high performance liquid chromatography, nuclear magnetic resonance spectroscopy and Fourier-transform infrared spectroscopy. The aim of this study was to develop and validate a short method for quantifying glycolaldehyde in aqueous solutions using liquid injection gas chromatography - mass spectrometry. Various chromatographic parameters were optimized to obtain a baseline separation of glycolaldehyde to other polar matrix components in the mixture as well as having a high peak symmetry, low band broadness and high resolution. The final gas chromatographic method consists of: hundred-fold dilution of the sample in acetonitrile, an initial oven temperature of 80 °C, mobile phase flow rate of 2 ml/min, a split ratio of 50:1, a thermal gradient of 60 °C/min, a final temperature of 220 °C, an injection volume of 1 µl, and free-fatty acid polyethylene glycol as the capillary stationary phase. The GA concentrations were determined through internal, external, standard addition and an internal standard corrected standard addition calibration curves. The developed method is rapid (5.3 min), accurate (>90%), precise (intra-day, inter-day and inter-laboratory precisions are all < 4% Relative Standard Deviation) with a limit of detection and a limit of quantification of 0.104 and 0.315 g/L, respectively. This method can be further optimized for the analysis of other carbohydrate related mixtures in aqueous solutions for both quantification and identification purposes.