Rapid determination of nitrate in vegetables by gas chromatography mass spectrometry

In this study we present a novel isotope dilution gas chromatography method for the determination of nitrate in vegetables. The analyte was extracted in water at 70 degrees C and mixed with N-15 isotopically enriched nitrate internal standard. The sample was centrifuged and the supernatant reacted with sulfamic acid for removal of nitrite, and with triethyloxonium tetrafluoroborate for converting nitrate into volatile EtONO2. This simple aqueous chemistry allowed for separation of analyte from sample matrix in the form of a gaseous derivative which could be sampled in the headspace before GC-MS analysis. This key-feature of the method made possible the collection of clean chromatograms within an elution time of only 1.8 min. Detection of EtONO2 could be performed using electron impact ionization with a standard GC-MS setup. The method was optimized and validated for the analysis of nitrate in fresh vegetables in the 10-10,000 mu g/g range with a detection limit of 2 mu g/g. Due to the use of primary isotope dilution quantitation, traceable results of high-precision were attained. (C) 2017 Published by Elsevier B.V.