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A Simple and Reliable HPTLC Method for the Quantification of the Intense Sweetener Sucralose®
(2003)
This paper describes a simple and fast thin layer chromatography (TLC) method for the monitoring of the relatively new intense sweetener Sucralose® in various food matrices. The method requires little or no sample preparation to isolate or concentrate the analyte. The Sucralose® extract is separated on amino‐TLC‐plates, and the analyte is derivatized “reagent‐free” by heating the developed plate for 20 min at 190°C. Spots can be measured either in the absorption or fluorescence mode. The method allows the determination of Sucralose® at the levels of interest regarding foreseen European legislation (>50 mg/kg) with excellent repeatability (RSD = 3.4%) and recovery data (95%).
Fluorescence Enhancement of Pyrene Measured by Thin-Layer Chromatography with Diode-Array Detection
(2003)
In-situ densitometry for qualitative or quantitative purposes is a key step in thin-layer chromatography. It offers a simple way of quantifying by measuring the optical density of the separated spots directly on the plate. A new TLC scanner has been developed which is able to measure TLC plates or HPTLC plates, at different wavelengths simultaneously, without destroying the plate surface. The system enables absorbance and fluorescence measurements in one run. Fluorescence measurements are possible without filters or other adjustments.
The measurement of fluorescence from a TLC plate is a versatile means of making TLC analysis more sensitive. Fluorescence measurements with the new scanner are possible without filters or special lamps. Improvement of the signal-to-noise ratio is achieved by wavelength bundling. During plate scanning the scattered light and the fluorescence are both emitted from the surface of the TLC plate and this emitted light provides the desired spectral information from substances on the TLC plate. The measurement of fluorescence spectra and absorbance spectra directly from a TLC plate is based on differential measurement of light emerging from sample-free and sample-containing zones.
The literature recommends dipping TLC plates in viscous liquids to enhance fluorescence. Measurement of the fluorescence and absorbance spectra of pyrene spots reveals the mechanism of enhancement of plate dipping in viscous liquids—blocked contact of the fluorescent molecules with the stationary phase or other sample molecules is responsible for the enhanced fluorescence at lower concentrations.
In conclusion, dipping in TLC analysis is no miracle. It is based on similar mechanisms observable in liquids. The measured TLC spectra are also very similar to liquid spectra and this makes TLC spec-troscopy an important tool in separation analysis.
Vorgestellt wird die Dioden-Array-Dünnschichtchromatographie als eine moderne und preiswerte Messmethode zur densitometrischen Erfassung von Substanzen auf einer DC- oder einer HPTLC-Platte. Sicher identifizierbar sind auch Substanzen mit schwachem Chromophor. Die Kubelka-Munk-Gleichung beschreibt einen linearen Zusammenhang zwischen Remissionslicht und lichtabsorbierender Stoffmenge auf der Platte. Die Auswertung im Spektralbereich von 316 bis 334 nm zeigt den Zusammenhang zwischen transformiertem Messsignal und aufgetragener Substanzmasse. Die schnelle Aufnahme von UV/vis-Spektren eröffnet der HPTLC den gesamten Bereich der Methodenvalidierung auf dem Niveau, auf welchem heute die HPLC-Analytik durchgeführt wird.
Quantitative Bestimmung von Clozapin im Serum mittels Dioden-Array Dünnschichtchromatographie
(2003)
The free convection in a vertical gap is generalized to realize new analytical solutions of the Boussinesq-equations. The steady and time-dependent solutions for the temperature and velocity distribution are discussed in detail depending on the mass flux in vertical direction. The range of existence for flows with and without back flow is obtained. The transient behaviour of the solutions during the time-dependent development displays interesting physical behaviour.
The structure of the separation bubble that appears in the secondary meridional flow between two coaxially rotating spheres at low and finite Reynolds number (Re) is considered. The low Re analytical study was motivated by recognizing some errors in the analytical work on this problem by Arunachalam and Majhi (1987, Q. Jl Mech. Appl. Math., 40, 47) whilst the finite Re experimental study was motivated by the desire to observe the separation bubble in the laboratory. Though the finite Re experiments were performed in a confined apparatus, they exhibit the qualitative features of the low Re theoretical predictions for the axisymmetric separation bubble that encloses two toroidal vortices symmetrically disposed above and below the mid‐plane of sphere separation, but strong effects of confinement are apparent. The flows observed include (i) a wall‐attached bubble symmetric about the mid‐plane at low Re, (ii) symmetric free‐standing bubbles at moderate Re, and (iii) an asymmetric bubble with flow separating from one sphere and attaching to the support shaft between the spheres at sufficiently high Re.