Development and single-laboratory validation of an HPLC method for the determination of cyclamate sweetener in foodstuffs

M. J. Scotter, L. Castle, D. P T Roberts, R. MacArthur, P. A. Brereton, S. K. Hasnip, N. Katz

Research output: Contribution to journalArticlepeer-review

12 Citations (Scopus)


A method for the determination of cyclamate has been developed and single-laboratory validated for a range of foodstuffs including carbonated and fruit-juice drinks, fruit preserves, spreads, and dairy desserts. The method uses the peroxide oxidation of cyclamate to cyclohexylamine followed by derivatization with trinitrobenzenesulfonic acid and analysis by a modified reversed-phase high-performance liquid chromatography-ultraviolet light (HPLC-UV). Cycloheptylamine is used as an internal standard. The limits of detection were in the range 1-20 mg kg-1 and the analysis was linear up to 1300 mg kg-1 cyclamic acid in foods and up to 67 mg l-1 in beverages. Analytical recovery was between 82% and 123%, and results were recovery corrected. Precision was within experimentally predicted levels for all of the matrices tested and Horrat values for the combined standard uncertainty associated with the measurement of cyclamate between 0.4 (water-based drinks) and 1.7 (spreads). The method was used successfully to test three soft drink samples for homogeneity before analytical performance assessment. The method is recommended for use in monitoring compliance and for formal testing by collaborative trial.

Original languageEnglish
Pages (from-to)614-622
Number of pages9
JournalFood Additives and Contaminants - Part A Chemistry, Analysis, Control, Exposure and Risk Assessment
Issue number5
Publication statusPublished - 03 Dec 2009
Externally publishedYes


  • Artificial sweetener
  • Cyclamate
  • Cyclamic acid
  • E952
  • Food
  • Food additive
  • High-performance liquid chromatography (HPLC)
  • Intense sweetener
  • Proficiency testing

ASJC Scopus subject areas

  • Food Science
  • Health, Toxicology and Mutagenesis
  • Public Health, Environmental and Occupational Health
  • Toxicology
  • Chemistry(all)


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