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Previous studies of the hyphenation of gas chromatographic separation and spectrophotometric detection in the ultraviolet wavelength range between 168 and 330 nm showed a high potential for applications where the analysis of complex samples is required. Within this paper the development of a state-of-the-art detection system for compounds in the vapour phase is described, offering an improved behaviour compared to previous systems: Dependent on the requirements of established detection systems hyphenated with gas chromatography, the main components of the system have to be designed for optimum performance and reliability of the spectrophotometric detector: A deuterium lamp as a broadband light source has been selected for improved stability in the measurements. A new-type absorption cell based on fiber-optics has been developed considering the dynamic necessary to compete with existing techniques. In addition, the influence of the volume of the cell on the chromatogram needs to be analyzed. Tests for determining the performance of the absorption cell in terms of chemical and thermal influences have been carried out. A new spectrophotometer with adequate spectral resolution in the wavelength range, offering improved stability and dynamic for an efficient use in this application was developed. Furthermore, the influence of each component on the performance, reliability and stability of the sensor system will be discussed. An overview and outlook over the potential applications in the environmental, scientific and medical field will be given.
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.
In thin-layer chromatography, fiber-bundle arrays have been introduced for spectral absorption measurements in the UV-region. Using all-silica fiber bundles, the exciting light will be detected after re-emission on the plate with a fiberoptic spectrometer. In addition, fluorescence light can be detected which will be masked by the re-emitted light. Therefore, it is helpful to separate the absorption and fluorescence on the TLC-plate. A modified three-array assembly has been developed: using one array for detection, the two others are used for excitation with broadband band deuterium-light and with UV-LEDs adjusted to the substances under test. As an example, the quantification of glucosamine in nutritional supplements or spinach leaf extract will be described. Using simply heating of the amino-plate for derivation, the reaction product of Glucosamine can be detected sensitively either by light absorption or by fluorescence, using the new fiber-optic assembly. In addition, the properties of the new 3-row fiber-optic array and the commercially available UV-LEDs will be shown, in the interesting wavelength region for excitation of fluorescence, from 260 nm to 360 nm. The squint angle having an influence on coupling efficiency and spatial resolution will be measured with the inverse farfield method. Some properties of UV-LEDs for analytical applications will be described and discussed, too.
We will present the first example of a two-dimensional scanned TLC-plate, measured by use of a diode-array scanner. A spatial resolution of 250 µm was achieved on plate. The system provides real 2D fluorescence and absorption spectra in the wavelength-range from 190 to 1000 nm with a spectral resolution of greater than 1 nm. A mixture of 12 sulphonamides was separated by using a cyanopropyl-coated silica gel plate (Merck, 1.16464) with the solvent mix of methyl tert-butyl ether-methanol-dichloromethane-cyclohexane-NH3 (25%) (48:2:2:1:1, v/v) in the first and with a mixture of water-acetonitrile-dioxane-ethanol (8:2:1:1, v/v) in the second direction. Both developments were carried out over a distance of 70 mm. A separation number (spot capacity) of 259 was calculated. We discussed a new formula for its calculation in 2D-TLC separations. The drawback of this method is that measuring a 2D-TLC plate needs more than 3 h measurement time.
HPTLC (High Performance Thin Layer Chromatography) is a well known and versatile separation method which shows many advantages when compared to other separation techniques. The method is fast and inexpensive and does not need time-consuming pretreatments. For visualisation of the sample distribution on a HPTLC-plate we developed a new and sturdy HPTLC-scanner. The scanner allows simultaneous registrations of spectra in a range from 198 nm to 612 nm with a spectral resolution of better than 0.8 nm. The on-plate spatial resolution is better than 160 μm. The measurement of 450 spectra in one separation track does not need more than two minutes. The new diode-array scanner offers a fast survey over a TLC-separation and makes various chemometric applications possible. For compound identification a cross-correlation function is described to compare UV sample spectra with appropriate library data. The cross-correlation function herein described can also be used for purity testing. Unresolved peaks can be virtually separated by use of a least squares fit algorithm. In summary, the diode arry system delivers much more information than the commonly used TLC-scanner.