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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 the present study, in vitro toxicity as well as biopersistence and photopersistence of four artificial sweeteners (acesulfame, cyclamate, saccharine, and sucralose) and five antibiotics (levofloxacin, lincomycin, linezolid, marbofloxacin, and sarafloxacin) and of their phototransformation products (PTPs) were investigated. Furthermore, antibiotic activity was evaluated after UV irradiation and after exposure to inocula of a sewage treatment plant. The study reveals that most of the tested compounds and their PTPs were neither readily nor inherently biodegradable in the Organisation for Economic Co-operation and Development (OECD)-biodegradability tests. The study further demonstrates that PTPs are formed upon irradiation with an Hg lamp (UV light) and, to a lesser extent, upon irradiation with a Xe lamp (mimics sunlight). Comparing the nonirradiated with the corresponding irradiated solutions, a higher chronic toxicity against bacteria was found for the irradiated solutions of linezolid. Neither cytotoxicity nor genotoxicity was found in human cervical (HeLa) and liver (Hep-G2) cells for any of the investigated compounds or their PTPs. Antimicrobial activity of the tested fluoroquinolones was reduced after UV treatment, but it was not reduced after a 28-day exposure to inocula of a sewage treatment plant. This comparative study shows that PTPs can be formed as a result of UV treatment. The study further demonstrated that UV irradiation can be effective in reducing the antimicrobial activity of antibiotics, and consequently may help to reduce antimicrobial resistance in wastewaters. Nevertheless, the study also highlights that some PTPs may exhibit a higher ecotoxicity than the respective parent compounds. Consequently, UV treatment does not transform all micropollutants into harmless compounds and may not be a large-scale effluent treatment option.
HPTLC on amino plates, with simple heating of the plates for derivatization, has been used for quantification of glucosamine in nutritional supplements. On heating the plate glucosamine reacts to form a compound which strongly absorbs light between 305 and 330 nm, with weak fluorescence. The reaction product can be detected sensitively either by absorption of light or by fluorescence detection. The detection limit in absorption mode is approximately 25 ng per spot. In fluorescence mode a detection limit of 15 ng is achievable. A calibration plot for absorption detection is linear in the range 25 to 4000 ng glucosamine. The derivative formed from glucosamine by heating is stable for months, and the relative standard deviation is 1.64% for 600 ng glucosamine. The amounts of glucosamine found in nutritional supplements were in agreement with the label declarations.
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.
Thin-layer chromatography is a rapid and reliable working method for quantification of mycotoxins which is suitable for checking EC legislation aflatoxin limits for dried figs without an RP-18 pre-column cleaning step. We describe normal-phase chromatography on silica gel plates with 2.4:0.05:0.1:0.05 ( v/v ) methyl t -butyl ether-water-methanol-cyclohexane as mobile phase and reversed-phase chromatography on RP-18 plates with methanol-4% aqueous ZnSO 4 solution-ethyl methyl ketone 15:15:3 ( v/v ) as mobile phase. Sample pretreatment was by modified QuEChERS (Quick, Easy, Cheap, Effective, Rugged, Safe) extraction with tetrahydrofuran or acetone. NaCl was used as QuEChERS salt. Response was a linear function of amount chromatographed in the ranges 3 to 100 pg per zone for aflatoxins B 2 and G 2 , 10 to 350 pg per zone for the aflatoxins B 1 and G 1 , and 0.25 to 2.5 ng per zone for ochratoxin A. Quantification limits for the aflatoxins were between 13 and 35 pg per zone (equivalent to 1.5 and 2.4 ppb, taking the pre-treatment procedure into account). Ochratoxin A was detectable with a limit of quantification of 970 pg per zone, corresponding to 56 ppb in the sample. Normal phase and RP-18 separations work rapidly, reliably, and at low cost. They are also suitable for checking the content of the mycotoxins patulin, penicillic acid, zearalenone, and deoxynivalenol.
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.
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.
We report improved separation of the highly toxic contact herbicides paraquat, diquat, difenzoquat, mepiquat, and chloromequat by HPTLC. Quantification was based on a new derivatization reaction using sodium tetraphenylborate. Measurements were in the wavelength range from 440 to 480 nm or from 440 to 590 nm. An LED emitting very intense light at 365 nm was used for excitation. The quantification limits of paraquat and diquat in water, using improved solid-phase extraction, was in the low ng L −1 range. The linear range covered more than two orders of magnitude. Recovery was investigated for all the compounds, and was insufficient, ranging from 11 to 92%, but the method is inexpensive, rapid, and works reliably.
Enzyme‐assisted HPTLC method for the simultaneous analysis of inositol phosphates and phosphate
(2023)
Background
The analysis of myo‐inositol phosphates (InsPx) released by phytases during phytic acid degradation is challenging and time‐consuming, particularly in terms of sample preparation, isomer separation, and detection. However, a fast and robust analysis method is crucial when screening for phytases during protein engineering approaches, which result in a large number of samples, to ensure reliable identification of promising novel enzymes or target variants with improved characteristics, for example, pH range, thermal stability, and phosphate release kinetics.
Results
The simultaneous analysis of several InsPx (InsP1‐InsP4 and InsP5 + 6) as well as free phosphate was established on cellulose HPTLC plates using a buffered mobile phase. Inositol phosphates were subsequently stained using a novel enzyme‐assisted staining procedure. Immobilized InsPx were hydrolyzed by a phytase solution of Quantum® Blueliquid 5G followed by a molybdate reagent derivatization. Resulting blue zones were captured by DAD scan. The method shows good repeatability (intra‐day and intra‐lab) with maximum deviations of the Rf value of 0.01. The HPTLC method was applied to three commercially available phytases at two pH levels relevant to the gastrointestinal tract of poultry (pH 5.5 and pH 3.6) to observe their phytate degradation pattern and thus visualize their InsPx fingerprint.
Conclusion
This HPTLC method presents a semi‐high‐throughput analysis for the simultaneous analysis of phytic acid and the resulting lower inositol phosphates after its enzymatic hydrolysis and is also an effective tool to visualize the InsPx fingerprints and possible accumulations of inositol phosphates.
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!
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.
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.
BioPower
(2009)
Das Projekt BioPower ist eine Kooperation des Instituts für Angewandte Forschung (IAF) der Hochschule Offenburg mit dem Institut für Mikrosystemtechnik (IMTEK) der Universität Freiburg. Es handelt sich um den Versuch, die im Körper vorhandenen Energiequellen sozusagen direkt anzuzapfen, um sie für technische Zwecke zu nutzen. Von den vielen bestehenden Möglichkeiten konzentriert sich die Forschung hier auf die Nutzung der Glukose im Blut, die auch sonst als Energieträger zur Versorgung der Zellen im Körper dient.
We present an improved quantification method for urethane found in spirits. The quantification is based on a derivatization reaction using cinnamaldehyde in combination with phosphoric acid. Measurements were carried out in the wavelength range from 445 to 460 nm using a diode-TLC device. An LED was used for illumination purposes. It emits very dense light at 365 nm. The quantification range of urethane is in the lower ng range. By applying 20 µL of sprits, the urethane quantification range is from 320 µg/L to 8.1 mg urethane per litre of spirit. The range of linearity covers nearly two magnitudes. The method is cheap, fast and reliable, and is able to monitor all European legislation limits without time-consuming sample pre-treatments.