Determination of cyclamate in artificial sweeteners and beverages using headspace single-drop microextraction and gas chromatography flame-ionisation detection

A new method for determination of cyclamate was developed using headspace single-drop microextraction (HS-SDME) and gas chromatography (GC). The method is based on the reaction of cyclamate and nitrite in the acidic media and microextraction of cyclohexene formed for subsequent determination with GC. Conditions for both derivatisation and HS-SDME have been optimised. The calibration curve for cyclamate determination showed good linearity in the range of 30–1000 μmol L⁻¹ (R² = 0.9992) and the limit of detection (S/N = 3) was estimated to be 5 μmol L⁻¹. The repeatability and reproducibility for a 200 μmol L⁻¹ of cyclamate were 4% and 4.8% (N = 5), respectively. The purposed method was successfully applied for determination of cyclamate in beverages and sweetener tablets. The average recovery of spiked samples was 97%. The results demonstrated that the developed method is simple, rapid, inexpensive, accurate and remarkably free from interference effects.