Determination of Sucralose in Soft Drinks by High-Performance Thin-Layer Chromatography: Interlaboratory Study
Abstract:An interlaboratory comparison was carried out to evaluate the effectiveness of a method based on HPTLC in which reagent-free derivatization is followed by UV/fluorescence detection. The method was tested for the determination of sucralose (C12H19Cl3O8; (2R,3R,4R,5S,6R)-2- [(2R,3S,4S,5S)-2,5-bis(chloromethyl)-3,4-dihydroxyoxolan- 2-yl]oxy-5-chloro-6-hydroxymethyl)oxane-3, 4-diol; CAS Registry No. 56038-13-2) in carbonated and still beverages at the proposed European regulatory limits. For still beverages, a portion of the sample was diluted with methanolwater. For carbonated beverages, a portion of the sample was degassed in an ultrasonic bath before dilution. Turbid beverages were filtered after dilution through an HPLC syringe filter. The separation of sucralose was performed by direct application on amino-bonded (NH2) silica gel HPTLC plates (no cleanup needed) with the mobile phase acetonitrilewater. Sucralose was determined after reagent-free derivatization at 190C; it was quantified by measurements of both UV absorption and fluorescence. The samples, both spiked and containing sucralose, were sent to 14 laboratories in five different countries. Test portions of a sample found to contain no sucralose were spiked at levels of 30.5, 100.7, and 299 mg/L. Recoveries ranged from 104.3 to 124.6 and averaged 112 for determination by UV detection; recoveries ranged from 98.4 to 101.3 and averaged 99.9 for determination by fluorescence detection. On the basis of the results for spiked samples (blind duplicates at three levels), as well as sucralosecontaining samples (blind duplicates at three levels and one split level), the values for the RSDr ranged from 10.3 to 31.4 for determinations by UV detection and from 8.9 to 15.9 for determinations by fluorescence detection. The values for the RSDR values ranged from 13.5 to 31.4 for determinations by UV detection and from 8.9 to 20.7 for determinations by fluorescence detection.
Document Type: Research Article
Affiliations: 1: European CommissionJoint Research Centre, Institute for Reference Materials and Measurements, Food Safety and Quality Unit, Retieseweg 111, B-2440 Geel, Belgium. 2: University of Applied Science Offenburg, Badstrasse 24, D-77652 Offenburg, Germany.
Publication date: July 1, 2009
- 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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