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Alle Materie strebt nach maximaler Unordnung. Diese Erkenntnis wird durch die thermodynamische Funktion der Entropie beschrieben. Auch bei jeglicher Art menschlichen Handelns wird die Entropie immer erhöht. Wird in der Technik Materie in geordnete Formen gebracht (z. B. beim Herstellen von Pfandflaschen), findet in diesem Produkt eine Entropieerniedrigung statt. Gleichzeitig wird aber an anderer Stelle die Unordnung beträchtlich vergrößert. Diese Entropieerhöhung nennen wir Abfall. Jede Entropieerhöhung ist mit dem Verbrauch wertvoller Ressourcen verbunden. Durch eine optimale Recyclingtechnik kann einer Entropieerhöhung von Materie entgegengearbeitet werden. Aber nur Recyclingraten von über 90 % erlauben eine wirksame Streckung der Ressourcen.
Vorrichtung (2) zur Analyse von Urin, umfassend: – eine Zuführ- und Abführeinrichtung (7), welche zur Zuführung einer bestimmten Urinmenge in eine wenigstens einen Analysebereich (8) aufweisende Analysekammer (9) eines Urinteststreifens (10) und zur Abführung einer bestimmten Urinmenge aus einer wenigstens einen Analysebereich (8) aufweisenden Analysekammer (9) eines Urinteststreifens (10) eingerichtet ist, wobei die Zuführ- und Abführeinrichtung (7) wenigstens ein bewegbar gelagertes Zuführ- und/oder Abführelement (28, 29) zum Zuführen einer bestimmten Urinmenge in einen Zuführbereich (33) der Analysekammer (9) des Urinteststreifens (10) und/oder zum Abführen einer bestimmten Urinmenge aus einem Abführbereich (34) der Analysekammer (9) des Urinteststreifens (10) aufweist, und – eine Erfassungseinrichtung (11), welche zur Erfassung einer zumindest abschnittsweisen Änderung wenigstens eines optisch erfassbaren Parameters, welcher sich in Abhängigkeit der Zusammensetzung einer diesen kontaktierenden Urinmenge optisch erfassbar verändert, des oder eines entsprechenden Analysebereichs (8) des oder eines entsprechenden Urinteststreifens (10) sowie zur Erzeugung einer Erfassungsinformation, welche wenigstens einen optisch erfassten Parameter des oder eines entsprechenden Analysebereichs (8) oder eine Änderung eines solchen beschreibt, eingerichtet ist.
Vorrichtung (2) zur Analyse von Urin, umfassend: – eine Zuführ- und Abführeinrichtung (7), welche zur Zuführung einer bestimmten Urinmenge in eine wenigstens einen Analysebereich (8) aufweisende Analysekammer (9) eines Urinteststreifens (10) und zur Abführung einer bestimmten Urinmenge aus einer wenigstens einen Analysebereich (8) aufweisenden Analysekammer (9) eines Urinteststreifens (10) eingerichtet ist, wobei die Zuführ- und Abführeinrichtung (7) wenigstens ein bewegbar gelagertes Zuführ- und/oder Abführelement (28, 29) zum Zuführen einer bestimmten Urinmenge in einen Zuführbereich (33) der Analysekammer (9) des Urinteststreifens (10) und/oder zum Abführen einer bestimmten Urinmenge aus einem Abführbereich (34) der Analysekammer (9) des Urinteststreifens (10) aufweist, und – eine Erfassungseinrichtung (11), welche zur Erfassung einer zumindest abschnittsweisen Änderung wenigstens eines optisch erfassbaren Parameters, welcher sich in Abhängigkeit der Zusammensetzung einer diesen kontaktierenden Urinmenge optisch erfassbar verändert, des oder eines entsprechenden Analysebereichs (8) des oder eines entsprechenden Urinteststreifens (10) sowie zur Erzeugung einer Erfassungsinformation, welche wenigstens einen optisch erfassten Parameter des oder eines entsprechenden Analysebereichs (8) oder eine Änderung eines solchen beschreibt, eingerichtet ist.
Vorrichtung (2) zur Analyse von Urin, umfassend: – eine Zuführ- und Abführeinrichtung (7), welche zur Zuführung einer bestimmten Urinmenge in eine wenigstens einen Analysebereich (8) aufweisende Analysekammer (9) eines Urinteststreifens (10) und zur Abführung einer bestimmten Urinmenge aus einer wenigstens einen Analysebereich (8) aufweisenden Analysekammer (9) eines Urinteststreifens (10) eingerichtet ist, wobei die Zuführ- und Abführeinrichtung (7) wenigstens ein bewegbar gelagertes Zuführ- und/oder Abführelement (28, 29) zum Zuführen einer bestimmten Urinmenge in einen Zuführbereich (33) der Analysekammer (9) des Urinteststreifens (10) und/oder zum Abführen einer bestimmten Urinmenge aus einem Abführbereich (34) der Analysekammer (9) des Urinteststreifens (10) aufweist, und – eine Erfassungseinrichtung (11), welche zur Erfassung einer zumindest abschnittsweisen Änderung wenigstens eines optisch erfassbaren Parameters, welcher sich in Abhängigkeit der Zusammensetzung einer diesen kontaktierenden Urinmenge optisch erfassbar verändert, des oder eines entsprechenden Analysebereichs (8) des oder eines entsprechenden Urinteststreifens (10) sowie zur Erzeugung einer Erfassungsinformation, welche wenigstens einen optisch erfassten Parameter des oder eines entsprechenden Analysebereichs (8) oder eine Änderung eines solchen beschreibt, eingerichtet 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.
We present a two-dimensional (2D) planar chromatographic separation method for phytoestrogenic active compounds on RP-18 W (Merck, 1.14296) phase. It could be shown that an ethanolic extract of liquorice (Glycyrrhiza glabra) roots contains four phytoestrogenic active compounds. As solvent, in the first direction, the mix of hexane, ethyl acetate, and acetone (45:15:10, v/v) was used, and, in the second direction, that of acetone and water (15:10, v/v) was used. After separation, a modified yeast estrogen screen (YES) test was applied, 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 inducing the reporter gene lacZ which encodes the enzyme β-galactosidase. This enzyme activity is determined on plate by using the fluorescent substrate MUG (4-methylumbelliferyl-β-d-galactopyranoside). The enzyme can also hydrolyse X-β-Gal (5-bromo-4-chloro-3-indoxyl-β-d-galactopyranosid) into β-galactose and 5-bromo-4-chloro-3-indoxyl. The indoxyl compound is oxidized by oxygen forming the deep-blue dye 5,5β-dibromo-4,4β-dichloro-indigo which allows to detect phytoestrogenic activity more specific in the presence of native fluorescing compounds.
We present a two-dimensional (2D) planar chromatographic separation of estrogenic active compounds on RP-18 W (Merck, 1.14296) phase. A mixture of 8 substances was separated using a solvent mix consisting of hexane, ethyl acetate, acetone (55:15:10, v/v) in the first direction and of acetone and water (15:10, v/v) in the second direction. Separation was performed on an RP-18 W plate over a distance of 70 mm. 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 inducing the reporter gene lacZ which encodes the enzyme β-galactosidase. This enzyme activity is determined on plate by using the fluorescent substrate MUG (4-methylumbelliferyl-β-d-galactopyranoside).
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.
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.
The main focus of this chapter is the theoretical and instrumental processes that underpin densitometric methods widely used in thin-layer chromatography (TLC). Densitometric methods include UV–vis, luminescence, and fluorescence optical measurements as well as infrared and Raman spectroscopic measurements. The chapter is divided in two general parts: a theoretical part and a practical part. The systems for direct radioactivity measurements and the combination of TLC with mass spectrometry are also discussed. All these systems allow measuring an intensity distribution directly on a TLC plate. We call this “in situ detection” because no analyte is removed from the plate.
The main focus of this chapter is the theoretical and instrumental processes that underpin densitometric methods widely used in thin-layer chromatography (TLC). Densitometric methods include UV–vis, luminescence and fluorescence optical measurements as well as infrared and Raman spectroscopic measurements. The chapter is divided in two general parts: a theoretical part and a practical part. The systems for direct radioactivity measurements and the combination of TLC with mass spectrometry are also discussed. All these systems allow measuring an intensity distribution directly on a TLC plate. We call this “in situ detection” because no analyte is removed from the plate.
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.
Improved separation of highly toxic contact herbicides paraquat (1,1′-dimethyl-4-4′-bipyridinium), diquat (6,7-dihydrodipyridol[ 1,2-a:2′,1′-c]pyrazine-5,8-di-ium), difenzoquat (1,2-dimethyl-3,5-diphenyl-1H-pyrazolium-methyl sulfate), mepiquat (1,1-dimethyl-piperidinium), and chloromequat (2-chloroethyltrimethylammonium) were presented by high-performance thin-layer chromatography (HPTLC). The quantification is based on a derivatization reaction, using sodium tetraphenylborate. Measurements were made in the wavelength range from 500 to 535 nm, using a light-emitting diode (LED) for excitation purposes, which emits very dense light at 365 nm. For calculations, a new theory of standard addition method was used, thus leading to a minimal error if exactly the same amount of sample content is added as a standard. The method provides a fast and inexpensive approach to quantification of the five most important quats used for plant protection purposes. The method works reliably because it takes into account losses during pre-treatment procedure. The method meets the European legislation limits for paraquat and diquat in drinking water according to United States Environmental Protection Agency (US EPA) method 549.2 which are 680 ng L−1 for paraquat and 720 ng L−1 for diquat. The method of standard addition in planar chromatography can be beneficially used to reduce systematic errors. Although recovery rates of 33.7% to 65.2% are observed, calculated contents according to the method of standard addition lie between 69% and 127% of the theoretical amounts.
We present a video-densitometric quantification method for the pain killer known as diclofenac and ibuprofen. These non-steroidal anti-inflammatory drugs were separated on cyanopropyl bonded plates using CH2Cl2, methanol, cyclohexane (95 + 5 + 40, v/v) as mobile phase. The quantification is based on a bio-effective-linked analysis using Vibrio fisheri bacteria. Within 10 min a CCD-camera registered the white light of the light-emitting bacteria. Diclofenac and ibuprofen effectively suppressed the bacterial light emission which can be used for quantification within a linear range of 10 to 2000 ng. The detection limit for ibuprofen is 20 ng and the limit of quantification 26 ng per zone. Measurements were carried out using a 16-bit ST-1603ME CCD camera with 1.56 megapixels (from Santa Barbara Instrument Group, Inc., Santa Barbara, USA). The range of linearity covers more than two magnitudes because the extended Kubelka-Munk expression is used for data transformation. The separation method is inexpensive, fast, and reliable.
High-performance thin-layer chromatography (HPTLC), as the modern form of TLC (thin-layer chromatography), is suitable for detecting pharmaceutically active compounds over a wide polarity range using the gradient multiple development (GMD) technique. Diode-array detection (DAD) in conjunction with HPTLC can simultaneously acquire ultraviolet‒visible (UV‒VIS) and fluorescence spectra directly from the plate. Visualization as a contour plot helps to identify separated zones. An orange peel extract is used as an example to show how GMD‒DAD‒HPTLC in seven different developments with seven different solvents can provide an overview of the entire sample. More than 50 compounds in the extract can be separated on a 6-cm HPTLC plate. Such separations take place in the biologically inert stationary phase of HPTLC, making it a suitable method for effect-directed analysis (EDA). HPTLC‒EDA can even be performed with living organism, as confirmed by the use of Aliivibrio fischeri bacteria to detect bioluminescence as a measure of toxicity. The combining of gradient multiple development planar chromatography with diode-array detection and effect-directed analysis (GMD‒DAD‒HPTLC‒EDA) in conjunction with specific staining methods and time-of-flight mass spectrometry (TOF‒MS) will be the method of choice to find new chemical structures from plant extracts that can serve as the basic structure for new pharmaceutically active compounds.
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.
Rudolf E. Kaiser
(2020)
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.
Wir präsentieren die weltweit erste Auswertung einer zweidimensional entwickelten HPTLC-Platte (2D-HPTLC) mit Hilfe eines Diodenarray Scanners. Das System erreicht eine räumliche Plattenauflösung von 250 µm. Es können Absorptions- und Fluoreszenzspektren im Wellenlängenbereich von 190 bis 1000 nm mit einer spektralen Auflösung von besser als 1 nm gemessen werden. Eine Trennzahl von 259 wurde erreicht. Damit zeigt die Methode bessere Trenneigenschaften als die meisten HPLC-Systeme. Der Nachteil der 2D-Auswertung ist der hohe Zeitbedarf von über 3 Stunden für eine Plattenmessung.
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
Die quantitative Dünnschichtchromatographie (HPTLC) mit einem Graustufen-Handscanner ist eine preiswerte, schnelle und präzise Methode zur Schwermetallbestimmung. Als Alternative zu teuren Densitometern wird ein Grünlichtscanner mit einer Auflösung von 256 Graustufen benutzt. Die Ortsauflösung beträgt maximal 400 dpi (dots per inch). Die Chromatogramme werden mit 300 dpi aufgenommen. Zur Entwicklung wird eine Camag-Linearkammer verwendet. Zur Probenvorbereitung werden die zu bestimmenden Schwermetallionen bei pH 4,2 mit Dithizon komplexiert. Nur die Metallkationen Zn(2+), Co(2+), Hg(2+), Cd(2+) und Ni(2+) reagieren zu einem farbigen Metallkomplex, wobei sich Zn(2+)- und Co(2+)-Komplexe chromatographisch abtrennen lassen. Nach Komplexierung der Wasserprobe wird mit Essigsäureethylester ausgeschüttelt, Probe- und Standardlösung auf eine Platte aus Kieselgel SI-60 aufgetragen, mit Essigsäureethylester fokussiert und nach der Trocknung der Platte mit Toluol entwickelt. Die HPTLC-Platte wird mit scannereigener Software eingelesen und im PCX-Format (PC PaintBrusch der Fa. ZSoft) auf die Festplatte abgelegt. Zur Auswertung wird eine Leseroutine benutzt. Die ganze Chromatographiebahn ist mit 150 Einzeldioden aufgenommen, die eine Strecke von 48 mm in 564 Einzelmessungen auflösen. Die Summe aller 150 Einzelaufnahmen liefert das Densitogramm aus dem der Schwermetallgehalt bestimmt wird.
Quantitative Bestimmung von Clozapin im Serum mittels Dioden-Array Dünnschichtchromatographie
(2003)
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 video-densitometric quantification method for the pain killer known as diclofenac and ibuprofen. These non-steroidal anti-inflammatory drugs were separated on cyanopropyl bonded plates using CH2Cl2, methanol, cyclohexane (95+5+40, v/v) as mobile phase. The quantification is based on a bio-effective-linked analysis using vibrio fischeri bacteria. Within 10 minutes a CCD-camera registers the white light of the light-emitting bacteria. Diclofenac and ibuprofen effectively suppress the bacterial light emission which can be used for quantification within a linear range of 10 to 2000 ng. The detection limit for ibuprofen is 20 ng and the limit of quantification 26 ng per zone. Measurements were carried out using a 16-bit ST-1603ME CCD camera with 1.56 megapixels [from Santa Barbara Instrument Group, Inc., Santa Barbara, USA]. The range of linearity covers more than two magnitudes because the extended Kubelka-Munk expression is used for data transformation [1]. The separation method is inexpensive, fast and reliable. Ibuprofen is named after its chemical description: iso-butyl-propanoic phenolic acid. Both pain killers are world-widein use and both substances are stable in aqueous solution. Both substances are mainly excreted in the urine.
Quantification of astaxanthin in salmons by chemiluminescence and absorption after TLC separation
(2018)
Astaxanthin is a keto-carotenoid, belongs to the chemical class of terpenes and is a yellow lipid soluble compound. The compound is present in marine animals like salmons and crustacean. Its colour is due to conjugated double bonds and these double bonds are responsible for its antioxidant effect. Its antioxidant activity is ten times stronger than other carotenoids and nearly 500 fold stronger than vitamin-E. We present a new thin layer chromatography (TLC) method to measure astaxanthin on TLC-plates (Merck, 1.05554) in the visible absorption range as well as by using chemiluminescence. For separation a solvent mixture of cyclohexane and acetone (10 + 2.4, v/v) was used. The RF-value of astaxanthin is 0.14.The limit of detection in vis-absorption is 64 ng / band and the limit of quantification is 92 ng/band. In chemiluminescence the values are 90 ng / band and 115 ng/band. The method offers two independently working measurement modes on a single plate which increase the accuracy of the quantification.
A new diode-array scanner in combination with a computer-controlled application system meets all the demands of modern HPTLC measurement. Automatic application, simultaneous measurements at different wavelengths, and different linearization models enable appropriate evaluation of all analytical questions. The theory of error propagation recommends quantification at reflectance values smaller than 0.8; this can be verified only by use of diode-array scanning. The same theory also recommends quantification by use of peak height data, because the theory predicts best precision only for peak height evaluation. Diode-array scanning with reflectance monitoring enables appropriate validation in TLC and HPTLC analysis. All these aspects result in substantial improvement of in-situ quantitative densitometric analysis, and simultaneous recording at different wavelengths opens the way for chemometric evaluation, e.g. peak purity monitoring, which improves the accuracy and reliability of HPTLC analysis.
Es wird ein Verfahren zur Herstellung eines nicht geschäumten porösen monolithischen oder faserförmigen Produkts aus anorganischem Polymer beschrieben, bei dem Wasserglas mit einem Carbonat und/oder Amid in bestimmten Mengen in Gegenwart von Wasser gehärtet wird. Außerdem werden monolithische Chromatographiesäulen und -platten, geträgerte Metall-Katalysatoren und Vliese beschrieben.
Poröse Massen oder Formkörper aus anorganischen polymeren und deren Herstellung (WO002014127762A1)
(2014)
Es wird ein Verfahren zur Herstellung einer porösen Masse oder eines porösen Formkörpers aus anorganischem Polymer beschrieben, bei dem Wasserglas mit einem Carbonat in bestimmten Mengen gehärtet wird und dabei verschiedene weitere Stoffe zugesetzt werden können. Außerdem werden poröse Massen und Formkörper, die mit diesem Verfahren erhältlich sind, beschrieben und deren Verwendung.
Poröse Massen oder Formkörper aus anorganischen polymeren und deren Herstellung (EP000002958875A1)
(2015)
We present a planar chromatographic separation method for the compounds caffeine, artemisinin, and equol, separated on high-performance thin-layer chromatography (HPTLC) silica gel plates. As solvents for separation, methyl t-butyl ether and cyclohexane (1:1, V/V) have been used for equol, cyclohexane and ethyl acetate (7:3, V/V) for artemisinin, and ethyl acetate and acetone (7:3, V/V) for caffeine. After separation, the plate was scanned with a very specific time of flight-direct analysis in real time-mass spectrometry (TOF-DART-MS) system using the (M + 1)+ signals of equol, artemisinin, and caffeine. The (M + 1) peak of artemisinin at 283.13 m/z is clearly detectable, which is the proof that DART-MS is applicable for the quantitative determination of rather instable molecules. The planar set-up of DART source, HPTLC plate and detector inlet in a line showed higher sensitivities compared to desorption at an angle. The optimal detector voltage increases with the molar mass of the analyte, thus an individual determination of optimal detector voltage setting for the different analyte is recommended to achieve the best possible measurement conditions. In conclusion, DART-MS detection in combination with an HPTLC separation allows very specific quantification of all three compounds.
Two solvent mixtures for high-performance thin-layer chromatographic (HPTLC) separation of some compounds showing estrogenic activity in the yeast estrogen screen (YES) assay are presented. The new method, planar yeast estrogen screen (pYES) combines the YES assay and a chromatographic separation on silica gel HPTLC plates with the performance of the YES assay. For separation, the analytes were applied bandwise to HPTLC plates (10 × 20 cm) with fluorescent dye (Merck, Germany). The plates were developed in a vertical developing chamber after 30 min of chamber saturation over a separation distance of 70 mm, using cyclohexane‒methyl-ethyl ketone (2:1, V/V) or cyclohexane‒CPME (3:2, V/V) as solvents. Both solvents allow separation of estriol, daidzein, genistein, 17β-estradiol, 17α-ethinyl estradiol, estrone, 4-nonylphenol and bis(2-ethylhexyl) phthalate.
A diode array HPTLC method for dequalinium chloride in pharmaceutical preparations is presented. For separation a Nano TLC silica gel plate (Merck) is used with the mobile phase methanol-7.8% aqueous NH(4)(+)CH(3)COO(-) (17:3, v/v) over a distance of 6 cm. Dequalinium chloride shows an R(F) value of 0.58. Pure dequalinium chloride is measured in the wavelength range from 200 to 500 nm and shows several by-products, contour plot visualized in absorption, fluorescence and using the Kubelka-Munk transformation. Scanning of a single track in absorption and fluorescence measuring 600 spectra in the range from 200 to 1100 nm takes 30s. As a sample pre-treatment of an ointment it is simply dissolved in methanol and can be quantified in absorption from 315 to 340 nm. The same separation can also be quantified using fluorescence spectrometry in the range from 355 to 370 nm. A new staining method for dequalinium chloride, using sodium tetraphenyl borate/HCl in water allows a fluorescence quantification in the range from 445 to 485 nm. The linearity range of absorption and fluorescence measurements is from 10 to 2000 ng. Sugar-containing preparations like liquids or lozenges with a reduced sample pre-treatment can be reliably quantified only in fluorescence. The total for the quantification of an ointment sample (measuring four standards and five samples), including all sample pre-treatment steps takes less than 45 min!
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 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.
The use of a TLC scanner can be regarded as a key step in high performance thin layer chromatography (HPTLC). Densitometric measurements transform the substance distribution on a TLC plate into digital computer data. Systems that allow quantitative measurements have been available for many years for either fluorescence or ultraviolet absorption measurements, while lately the reflection analysis mode for both types is the most common application. New scanning approaches are designed to aid the analyst who has common demands for TLC-densitometry without using special data, such as scanned images. Two examples that have been developed lately in the laboratories of the authors are described in this paper. These approaches were developed on the basis of current needs for analysts who employ TLC as a tool in research, as well as in routine analysis. One approach is aimed to support analysts in economically disadvantaged areas, where cost intensive apparatus is unsuitable but trace analysis by simple means is required. The other system, allows the spectral determination of chromatographic spots on TLC plates covering the ultraviolet and visible range, thus, revealing highly desired information for the analyst.
Thin-layer chromatography (TLC) is a well-established and widely used separation technique. Most undergraduate students of chemistry or food science used TLC as a primitive separation tool, which does not need more than small pieces of TLC plates, a glass jar and some solvents. TLC has evolved from a simple separation method of the past into an instrumental technique that offers automation, reproducibility and accurate quantification for a wide variety of applications [1]. The use of modern 10*10 cm TLC plates with narrow particle size distribution is called high performance thin layer chromatography (HPTLC), to distinguish the method from the use of traditional 20 20 cm TLC plates.
Limits of quantification of some neonicotinoid insecticides measured by thin-layer chromatography
(2012)
A simple method to quantify the neonicotinoid insecticides nitenpyram, thiamethoxam, acetamiprid, imidacloprid, thiacloprid and clothianidin directly on an HPTLC-plate is presented. As stationary phase silica gel 60 RP-18WF254 s plates were used and a mixture of methyl-t-butyl ether, 2-butanone, NH3 (25%) (5 + 2+0.1, v/v) was used as solvent. All neonicotinoid insecticides show light absorptions below 300 nm. The calculated limits of quantification (LOQ) by UV-detection are in the range from 12 ng to 26 ng on plate depending on the different insecticides.Nitenpyram can be stained using fast blue salt B, forming red zones. The observed LOQ is 25 ng on plate. Acetamiprid can be specifically stained using phenylglyoxylic acid forming a yellow/green fluorescent compound. The LOQ is 52 ng per spot.The compounds thiamethoxam, acetamiprid, thiacloprid and clothianidin can be transformed into blue fluorescing zones, using a relatively new staining solution. This consists of tetraphenylborate and HCl. This is the first publication mentioning that neonicotinoids undergo this reaction. The calculated limits of quantification are in the range from 10 ng to 27 ng on plate.A simple pre-treatment procedure using an acetonitrile extraction and a Chromabond SiOH clean up procedure leads to overall LOQs for bee samples of 48 to 108 µg/Kg. The method can be used to measure neonicotinoid contaminations of bees.
We present a planar chromatographic separation method for the phytoestrogenic active compound equol, separated on RP-18 W (Merck, 1.14296) phase. It could be shown that an ethanolic cattle manure extract contains this phytoestrogenic active compound to a larger amount. As solvents for the mobile phase, hexane, ethyl acetate, and acetone (45:15:10, v/v); acetone and water (15:10, v/v); and n-hexane, CH2Cl2, ethyl acetate, methanol, and formic acid (40:40:20:5:1, v/v) have been used. After separation, a modified yeast estrogen screen (YES) test was applied, using the yeast strain Saccharomyces cerevisiae BJ3505 containing an estrogen receptor. Its activation by equol induces the reporter gene lacZ which encodes the enzyme β-galactosidase. The enzyme activity is measured directly on the TLC plate by using the substrate MUG (4-methylumbelliferyl-β-d-galactopyranoside) or the substrate X-β-Gal (5-bromo-4-chloro-3-indoxyl-β-d-galactopyranoside). β-Galactosidase cleaves MUG into a fluorescing compound. X-β- Gal is also hydrolyzed and then oxidized by oxygen forming the deep-blue dye 5,5′-dibromo-4,4′-dichloro-indigo. Both reactions in combination with a thin-layer chromatography (TLC) separation allow very specific detecting of equol in cattle manure, although that is a very challenging matrix. Preliminary results show that the average content of equol in liquid manure is roughly 60 μg g−1. The value for urine is 50 μg mL−1.