Determination of Cyclamate in Foods by Ultraperformance Liquid Chromatography/Tandem Mass Spectrometry

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Abstract:

A highly sensitive and selective method that requires minimal sample preparation was developed for the confirmation and quantitation of cyclamate in a variety of foods by high-performance liquid chromatography/tandem mass spectrometry (HPLC/MS/MS). Sample preparation consisted of homogenization followed by extraction and dilution of cyclamate with water. HPLC separation was achieved using a bridged ethyl hybrid C18 high-pressure column with a mobile phase consisting of 0.15 acetic acid and methanol. Under electrospray ionization negative conditions, quantitation was achieved by monitoring the fragment m/z 79.7 while also collecting parent ion m/z 177.9. Two food matrixes, diet soda and jelly, were subjected to a validation procedure in order to evaluate the applicability of the method. The cyclamate limit of detection for both matrixes was determined to be 0.050 g/g with a limit of quantitation of 0.150 g/g. The correlation coefficient of the calibration curves was >0.9998 from 0.0005 to 0.100 g/mL. The method has been used for the determination of cyclamate in several foods and the results are presented.

Document Type: Research Article

Affiliations: New York State Department of Agriculture and Markets, Food Laboratory, Building 7, State Office Campus, Albany, NY 12235.

Publication date: September 1, 2008

More about this publication?
  • The Journal of AOAC INTERNATIONAL publishes refereed papers and reviews in the fields of chemical, biological and toxicological analytical chemistry for the purpose of showcasing the most precise, accurate and sensitive methods for analysis of foods, food additives, supplements and contaminants, cosmetics, drugs, toxins, hazardous substances, pesticides, feeds, fertilizers and the environment available at that point in time. The scope of the Journal includes unpublished original research describing new analytical methods, techniques and applications; improved approaches to sampling, both in the field and the laboratory; better methods of preparing samples for analysis; collaborative studies substantiating the performance of a given method; statistical techniques for evaluating data. The Journal will also publish other articles of general interest to its audience, e.g., technical communications; cautionary notes; comments on techniques, apparatus, and reagents.
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