GC-MS quantitation of isocitric acid in the presence of a large excess of citric acid

A GC-MS method has been developed for the analysis of the sugar and carboxylic acid content of citrus fruits, including the quantitation of isocitric acid in the presence of a large excess of citric acid. Optimum conditions have been determined for the analysis (from one solution, by one injection, on a 30 m DB-5 column) of the TMS oxime and/or TMS derivatives of sugars and acids obtained from various lemon, grapefruit, and orange samples. Quantitation was based on the monitoring of the total ion current and of selective fragments. The utility of the method has been demonstrated by the determination of isocitric acid in the presence of 10- to 200-fold excess of citric acid.