Automated In-Injector Derivatization Combined with High-Performance Liquid Chromatography–Fluorescence Detection for the Determination of Semicarbazide in Fish and Bread Samples

Semicarbazide (1) is a widespread genotoxic food contaminant originating as a metabolic byproduct of the antibiotic nitrofurazone used in fish farming or as a thermal degradation product of the common flour additive azodicarbonamide. The goal of this study is to develop a simple and sensitive high-performance liquid chromatography coupled with fluorescence detection (HPLC-FLD) method for the detection of compound 1 in food products. In comparison to existing methods for the determination of compound 1, the reported method combining online precolumn derivatization and HPLC-FLD is less labor-intensive, produces higher sample throughput, and does not require the use of expensive analytical instruments. After validation of accuracy and precision, this method was applied to determine the amount of compound 1 in fish and bread samples. Comparative studies using an established liquid chromatography coupled with tandem mass spectrometry method did not yield systematically different results, indicating that the developed HPLC-FLD method is accurate and suitable for the determination of compound 1 in fish and bread samples.