Open Access

Die Weltwirtschaftskrise 2008 hat mit ihrer zeitweisen Verknappung von Acetonitril eindringlich gezeigt, dass man nicht nur auf eine einzige chromatographische Methode setzten sollte. Genau dies wird aber im Augenblick getan, denn Industrie und Forschung setzen mehrheitlich auf die High Performance Liquid Chromatography (HPLC) als die Trennmethode ihrer Wahl. Für viele Anwendungen in der Pharmazie, in der Umweltanalytik, der Lebensmittelanalytik, aber auch in der Inprozesskontrolle gibt es mit der Dünnschichtchromatografie eine Alternative.

Diode-array planar chromatography is a versatile tool for identification of pharmaceutical substances In this paper thirty-three compounds with benzodiazepine properties were investigated and the separating conditions for silica gel HPTLC plates and three mobile phases were optimized. Diode-array HPTLC makes it possible to identify all the compounds with high certainty down to a level of 20 ng. An algorithm for spectral recognition which is combined with R F values from the three separation steps into one fit factor is presented. This set of data is unique for each of the compounds investigated and enables unequivocal identification. The method is rapid, inexpensive, and sensitive down to a level of 20 ng mL −1.

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.