Sensitive and precise voltammetric methods for the determination of trace amounts of furaldehydes, mainly as furfural (F) and 5-hydroxymethyl-2-furaldehyde (HMF), in foods, pharmaceutical and other matrices is described. Determination of total furaldehyde at < mg g À1 levels in alkaline buffered aqueous media was individually investigated. By the use of ordinary SWV and adsorptive square wave stripping voltammetry (Ad-SWSV), the detection limits for determination of F and HMF found to be 400 and 10 ng g À1 , respectively. At a 1.0 mg g À1 level of furfural in sample, the relative standard deviation (n ¼ 4) was 2.79%. The application of Ad-SWSV to the determination of F and HMF, after their in situ derivatization with trimethylaminoacetohydrazide chloride (Girards reagent T) at a static mercury drop electrode (SMDE) in NH 3 -NH 4 Cl buffer of pH 9.5, resulted in a limit of detection of 10 ng g À1 for the resolved peaks of HMF and F. The results obtained by the proposed method for the real samples were compared with the corresponding results from UV-spectrophotometry and HPLC experiments in various matrices.