Determination of free and reversibly-bound sulfite in selected foods by high-performance liquid chromatography with fluorometric detection.

A rapid and accurate method for measuring low part-per-million levels of free and reversibly-bound sulfites in selected foods by using high-performance liquid chromatography (HPLC) with fluorometric detection was developed. Sulfites were extracted with sodium tetrachloromercurate solution and determined by HPLC-fluorescence spectrometry. During the HPLC analysis, the sample extract was reacted with sodium hydroxide to liberate the reversibly-bound sulfite and subsequently separated from other interferences by a size exclusion column. The effluent was then reacted with o-phthalaldehydelammonium chloride reagent to form a fluorescing 1-sulfonatoisoindole derivative and analyzed by a fluorescence detector. The method has been applied to a variety of foods and food products, with no significant interference encountered in matrixes such as soy products, cabbage, broccoli, brassica, ginger, fungus, mushroom, mandarin peel, potato chips, and biscuits. It was shown to have a broad linear range of 0.01 to 0.4 mg/L as SO2. The spike recoveries of sodium sulfite, sodium metabisulfite, and formaldehyde-sodium bisulfite adduct at the 5 to 10 mg/kg level in the tested food matrix were within 80-120%, and the limit of detection was 5 mg/kg. Laboratory of Government Chemist Reference Material LGC7111 (potato powder) was used to assess the accuracy of the method. The expanded measurement uncertainty of the method at 95% confidence level was estimated to be 17%.