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We present a video-densitometric quantification method in combination with diode-array quantification for the methyl-, ethyl-, propyl-, and butylparaben in cosmetics. These parabens were separated on cyanopropyl bonded plates using water-acetonitrile-dioxane-ethanol-NH3 (25%) (8:2:1:1:0.05, v/v) as mobile phase. The quantification is based on UV-measurements at 255 nm and a bioeffectively-linked analysis using Vibrio fischeri bacteria. Within 5 min, a Tidas S 700 diode-array scanner (J&M, Aalen, Germany) scans 8 tracks and thus measures in total 5600 spectra in the wavelengths range from 190 to 1000 nm. The quantification range for all these parabens is from 20 to 400 ng per band, measured at 255 nm. In the V. fischeri assay a CCD-camera registers the white light of the light-emitting bacteria within 10 min. All parabens effectively suppress the bacterial light emission which can be used for quantifying within a linear range from 100 to 400 ng. Measurements were carried out using a 16-bit MicroChemi chemiluminescence system (biostep GmbH, Jahnsdorf, Germany), using a CCD camera with 4.19 megapixels. The range of linearity is achieved because the extended Kubelka-Munk expression was used for data transformation. The separation method is inexpensive, fast, and reliable.
We present a two dimensional (2D) planar chromatographic separation of estrogenic active compounds on RP-18 (Merck, 1.05559) and silica gel (Merck, 1.05721) phase. A mixture of 13 substances was separated using a solvent mix consisting of methanol–acetonitrile–water (2 + 2 + 1, v/v/v) on RP-18 phase in the first direction and cyclohexane–butylacetate–methanol (8 + 6 + 1, v/v/v) in the second direction on silica gel plate. Both developments were carried out over a distance of 70 mm. We used the grafted method to combine both plates in a 2D-separation. This 2D-separation method can be used to quantify 17α-ethinylestradiol (EE2) in an effect-directed analysis using the yeast strain Saccharomyces cerevisiae BJ3505. The test strain (according to McDonnell) contains the estrogen receptor. Its activation by estrogen active compounds is measured by inducting the reporter gene lacZ that encodes the enzyme ß-galactosidase. This enzyme activity is determined on plate by using the fluorescent substrate MUG (4-methylumbelliferyl ß-D-galactopyranoside).
Das einzige deutschsprachige Buch zur quantitativen Dünnschichtchromatographie auf dem Markt
Für Wissenschaftler und Anwender: von der vollständigen Behandlung der Theorie bis hin zu Entwicklungs- und Auswertetechniken
Auch für Einsteiger geeignet, da das Buch entsprechend der Arbeitsschritte einer DC-Analyse aufgebaut ist
A 2D-separation of 16 polyaromatic hydrocarbons (PAHs) according to the Environmental Protecting Agency (EPA) standard was introduced. Separation took place on a TLC RP-18 plate (Merck, 1.05559). In the first direction, the plate was developed twice using n-pentane at −20°C as the mobile phase. The mixture acetonitrile-methanol-acetone-water (12:8:3:3, v/v) was used for developing the plate in the second direction. Both developments were carried out over a distance of 43 mm. Further on in this publication, a specific and very sensitive indication method for benzo[a]pyrene and perylene was presented. The method can detect these hazardous compounds even in complicated PAH mixtures. These compounds can be quantified by a simple chemiluminescent reaction with a limit of detection (LOD) of 48 pg per band for perylene and 95 pg per band for benzo[a]pyrene. Although these compounds were separated from all other PAHs in the standard, a separation of both compounds was not possible from one another. The method is suitable for tracing benzo[a]pyrene and/or perylene. The proposed chemiluminescence screening test on PAHs is extremely sensitive but may indicate a false positive result for benzo[a]pyrene.
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.