Sampling and Analytical Method for Alpha-Dicarbonyl Flavoring Compounds via Derivatization with o-Phenylenediamine and Analysis Using GC-NPD

A novel methodology is described for the sampling and analysis of diacetyl, 2,3-pentanedione, 2,3-hexanedione, and 2,3-heptanedione. These analytes were collected on o-phenylenediamine-treated silica gel tubes and quantitatively recovered as the corresponding quinoxaline derivatives. After derivatization, the sorbent was desorbed in 3 mL of ethanol solvent and analyzed using gas chromatography/nitrogen-phosphorous detection (GC/NPD). The limits of detection (LOD) achieved for each analyte were determined to be in the range of 5–10 nanograms/sample. Evaluation of the on-tube derivatization procedure indicated that it is unaffected by humidities ranging from 20% to 80% and that the derivatization procedure was quantitative for analyte concentrations ranging from 0.1 μg to approximately 500 μg per sample. Storage stability studies indicated that the derivatives were stable for 30 days when stored at both ambient and refrigerated temperatures. Additional studies showed that the quinoxaline derivatives were quantitatively recovered when sampling up to a total volume of 72 L at a sampling rate of 50 cc/min. This method will be important to evaluate and monitor worker exposures in the food and flavoring industry. Samples can be collected over an 8-hour shift with up to 288 L total volume collected regardless of time, sampling rate, and/or the effects of humidity.