Development and single-laboratory validation of an improved method for the determination of cyclamate in foods using liquid chromatography/tandem mass spectrometry

Abstract

A fast and reliable LC-MS/MS method for the determination of cyclamate in a variety of food matrices was developed and validated. This method provides both quantitation and qualitative mass spectral determination important for analysis of regulatory samples. Utilization of a cyclamate-d11 internal standard corrects for potential matrix interferences during sample injection and allows minimal sample preparation. Seventeen commercially available food products were fortified at 250 μg/mL and tested as part of the method validation. Recoveries ranged from 72 to 110%, with RSDs ranging from 3 to 15%. The linear range spanned 0.010-1.00 μg/mL. LODs were 0.1 and 0.6 ng/mL, determined in pomegranate juice and dried fig, respectively. LOQs were 0.3 and 1.6 ng/mL, which are significantly lower than needed to measure cyclamate when used as a food additive. The interday and intraday accuracy and precision data are presented. This method was validated for analysis of a variety of commonly adulterated products, including drinks, dried fruits, jams, and hard candies.