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Phenolic compounds, such as flavonoids and phenolic acids, are very important substances that occur in various medicinal plants. They show different pharmacological activities which might be useful in the therapy of many diseases. Phenolic compounds have achieved an increasing interest over the last years because these compounds are easily oxidized and, thus, act as strong antioxidants. We present the chemiluminescence of different phenolic compounds measured directly on high-performance thin-layer chromatography LiChrospher® plates using the oxalic acid derivative bis(2,4,6-trichlorophenyl) oxalate (TCPO) in conjunction with H2O2. Our results indicate that chemiluminescence intensity increases with an ascending number of phenolic groups in the molecule. The method can be used to detect phenolic compounds in beverages like coffee, tea, and wine.
We present a videodensitometric quantification method for methadone in syrup, separated by thin-layer chromatography (TLC). The quantification is based on a derivation reaction with Dragendorf reagent. Measurements were carried out using a 16-bit flatbed scanner. The range of linearity covers two magnitudes of power using the Kubelka-Munk expression for data transformation. The separation method is inexpensive, fast, and reliable.
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.
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.
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.
In thin-layer chromatography the development step distributes the sample throughout the layer, a process which strongly affects the reflection signals. The essential requirement for quantitative thinlayer chromatography is not a constant sample concentration but constant sample distribution in each sample spot. This makes evaporation of the mobile phase extremely important, because all tracks of a TLC plate must be dried uniformly. This paper shows that quantitative TLC is possible even if the concentration of the sample is not constant throughout the layer or if the distribution of the sample is not known. With uniform sample distribution, classical Kubelka-Munk theory is valid for isotropic scattering only. In the absence of this constraint classical Kubelka-Munk theory must be extended to situations where scattering is asymmetric. This can be achieved by modification of the original Kubelka-Munk equation. Extended theory is presented which is not only capable of describing asymmetrical scattering in TLC layers but also includes a formula for absorption and fluorescence in diode-array TLC. With this new theory all different formulas for diode-array thin-layer chromatographic evaluation are combined in one expression.