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Gas chromatography-mass spectrometry method for determining the methanol and acetic acid contents of pectin using
Brett J Savary1, Alberto Nuñez
1Eastern Regional Research Center, Agricultural Research Service, US Department of Agriculture, 600 East Mermaid Lane, Wyndmoor, PA 19038, USA. bsavary@arserrc.gov
Abstract:
A simple, fast, and direct procedure was developed for the simultaneous determination of the methanol and acetic acid present as esters in the plant cell wall polysaccharide pectin. After base-hydrolysis of esters and acidification of pectin samples, headspace solid-phase microextraction (SPME) was performed using a Carboxen-PDMS fiber assembly. Methanol and acetic acid were separated by gas chromatography with a Chrompak PoraPlot Q capillary column and detected using electron impact mass spectrometry with selected ion monitoring. Stable deuterated isotopomers (d3-methanol and d3-acetic acid) were used as internal standards and for constructing calibration curves, providing accurate and absolute quantification of analytes. The methanol and acetic acid contents in 1 mg quantities of fruit and vegetable pectins were readily quantified by this procedure.
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