Determination of sucralose in soft drinks by high-performance thin-layer chromatography: interlaboratory study.
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 (C12H19C13O8; (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 methanol-water. 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 acetonitrile-water. Sucralose was determined after reagent-free derivatization at 190 degrees C; 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 sucralose-containing 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.
Stroka
Joerg
J
European Commission-Joint Research Centre, Institute for Reference Materials and Measurements, Food Safety and Quality Unit, Retieseweg 111, B-2440 Geel, Belgium. joerg.stroka@ec.europa.eu
Doncheva
Ivanka
I
Spangenberg
Bernd
B
D001628:Beverages / Q000032:analysis*; D002138:Calibration; D002855:Chromatography, Thin Layer; D007202:Indicators and Reagents; D012015:Reference Standards; D015203:Reproducibility of Results; D012996:Solutions; D013050:Spectrometry, Fluorescence; D013056:Spectrophotometry, Ultraviolet; D013395:Sucrose / Q000031:analogs & derivatives* / Q000032:analysis; D013549:Sweetening Agents / Q000032:analysis*
D007202:Indicators and Reagents; D012996:Solutions; D013549:Sweetening Agents; D013395:Sucrose; C026285:trichlorosucrose