Refine
Document Type
Conference Type
- Konferenzartikel (2)
Language
- English (5) (remove)
Has Fulltext
- no (5)
Is part of the Bibliography
- yes (5)
Keywords
- Faseroptik (5) (remove)
Institute
Open Access
- Closed Access (4)
- Open Access (1)
The identification and quantification of compounds in the gas phase becomes of increasing interest in the context of environmental protection, as well as in the analytical field. In this respect, the high extinction coefficients of vapours and gases in the ultraviolet wavelength region allow a very sensitive measurement system. In addition, the increased performance of the components necessary for setting up a measurement system, such as fibres, light sources and detectors has been improved. In particular the light sources and detectors offer improved stability, and the deep UV performance and solarisation resistance of fused silica fibres allow have been significantly optimized in the past years. Therefore a compact and reliable detection system with high measuring accuracy is developed. Within this paper possible applications of the system under development and recent results will be discussed.
HPTLC (High Performance Thin Layer Chromatography) is a well known and versatile separation method which shows a lot of advantages and options in comparison to other separation techniques. The method is fast and inexpensive and does not need time-consuming pretreatments. Using fiber-optic elements for controlled light-guiding, the TLC-method was significantly improved: the new HPTLC-system is able to measure simultaneously at different wavelengths without destroying the plate surface or the analytes on the surface. For registration of the sample distribution on a HPTLC-plate we developed a new and sturdy diode-array HPTLC- scanner which allows registration of spectra on the TLC- plates in the range of 198 nm to 610 nm with a spectral resolution better than 1.2 nm. The spatial resolution on plate is better than 160 micrometers . In the spectral mode, the new HPTLC-scanner delivers much more information than the commonly used TLC-scanner. The measurement of 450 spectra of one separation track does not need more than three minutes. However, in the fixed wavelength mode the contour plot can be measured within 15 seconds. In this case, the signal will be summarized and averaged over a spectral range having FWHM from 10 nm to 25 nm depending on the substance under test. The new diode-array HPTLC-scanner makes various chemometric applications possible. The new method can be used easily in clinical diagnostic systems easily, e.g. for blood and uring investigations. In addition, new applications are possible. For example, the rich structured PAHs were studied. Although the separation is incomplete the 16 compounds can be quantified using suitable wavelengths.
A systematic toxicological analysis procedure using high-performance thin layer chromatography in combination with fibre optical scanning densitometry for identification of drugs in biological samples is presented. Two examples illustrate the practicability of the technique. First, the identification of a multiple intake of analgesics: codeine, propyphenazone, tramadol, flupirtine and lidocaine, and second, the detection of the sedative diphenhydramine. In both cases, authentic urine specimens were used. The identifications were carried out by an automatic measurement and computer-based comparison of in situ UV spectra with data from a compiled library of reference spectra using the cross-correlation function. The technique allowed a parallel recording of chromatograms and in situ UV spectra in the range of 197–612 nm. Unlike the conventional densitometry, a dependency of UV spectra by concentration of substance in a range of 250–1000 ng/spot was not observed.
In-situ densitometry for qualitative or quantitative purposes is a key step in thin-layer chromatography (TLC). It is a simple means of quantification by measurement of the optical density of the separated spots directly on the plate. A new scanner has been developed which is capable of measuring TLC or HPTLC (high-performance thin-layer chromatography) plates simultaneously at different wavelengths without damaging the plate surface. Fiber optics and special fiber interfaces are used in combination with a diode-array detector. With this new scanner sophisticated plate evaluation is now possible, which enables use of chemometric methods in HPTLC. Different regression models have been introduced which enable appropriate evaluation of all analytical questions. Fluorescent measurements are possible without filters or special lamps and signal-to-noise ratios can be improved by wavelength bundling. Because of the richly structured spectra obtained from PAH, diode-array HPTLC enables quantification of all 16 EPA PAH on one track. Although the separation is incomplete all 16 compounds can be quantified by use of suitable wavelengths. All these aspects are enable substantial improvement of in-situ quantitative densitometric analysis.
In this paper a high-performance thin-layer chromatography (HPTLC) scanner is presented in which a special fibre arrangement is used as HPTLC plate scanning interface. Measurements are taken with a set of 50 fibres at a distance of 400 to 500 μm above the HPTLC plate. Spatial resolutions on the HPTLC plate of better than 160 μm are possible. It takes less than 2 min to scan 450 spectra simultaneously in a range of 198 to 610 nm. The basic improvement of the item is the use of highly transparent glass fibres which provide excellent transmission at 200 nm and the use of a special fibre arrangement for plate illumination and detection.