Cumulative CAMAG Bibliography Service CCBS

Our CCBS database includes more than 11,000 abstracts of publications. Perform your own detailed search of TLC/HPTLC literature and find relevant information.

The Cumulative CAMAG Bibliography Service CCBS contains all abstracts of CBS issues beginning with CBS 51. The database is updated after the publication of every other CBS edition. Currently the Cumulative CAMAG Bibliography Service includes more than 11'000 abstracts of publications between 1983 and today. With the online version you can perform your own detailed TLC/HPTLC literature search:

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      130 147
      Globotriaosylceramide-related biomarkers of Fabry disease identified in plasma by high-performance thin-layer chromatography – densitometry – mass spectrometry
      C. JARNE, L. MEMBRADO, M. SAVIRÓN, J. VELA, J. ORDUNA, R. GARRIGA, J. GALBÁN, V. L. CEBOLLA* (*Institute of Carbon Chemistry, Spanish National Research Council (CSIC), Saragossa, Spain; vcebolla@icb.csic.es)

      J Chromatogr A 1638, 461895 (2021). Samples were sphingolipid-rich fractions of unproteinated blood plasma from healthy humans or from Fabry’s disease patients, as well as standards of sphingomyelin (SM) and of globotriaosylceramides (Gb3 = ceramide trihexosides), and related compounds (lyso-ceramide trihexosides, lactosyl ceramide, glucosyl ceramide). HPTLC on silica gel (Lichrosphere with spherical particles) by automated multiple development with a 9-step gradient, starting with pure methanol and ending with dichloromethane – methanol 9:1. Visualization and densitometry under UV 190 nm. Derivatization for Gb3 and derivatives (but not for SM) by immersion into orcinol solution (0.2 %, with sulfuric acid 10 %), followed by 15 min heating at 100 °C and by densitometry under visible light 550 nm. Bands of interest were directly eluted with methanol from underivatized plates into an ion-trap MS, through the oval head of a TLC-MS interface (with stainless steel frit to remove silica gel particles). Two different ionization processes were used: (A) electrospray ionization (ESI, capillary voltage 4 kV, endplate offset voltage -0.5 kV, nebulizer pressure 40 psi, drying gas 9 mL/min at 350 °C); (B) atmospheric pressure chemical ionization (APCI, capillary voltage 2–3 kV, current intensity 4.5 µA, nebulizer pressure 45 psi, drying gas 5 mL/min at 350 °C; vaporization at 450 °C). Full MS spectra were recorded up to m/z 1500 in positive ion mode. The relative ion intensities were used to quantify the detected species. Previous to this study, the precision of the elution head positioning was tested on Gb3 standard zones, comparing 3 positions for analyte elution: from the centre and from each higher or lower side of the band. The same main m/z peaks were observed in the 3 positions, but in different proportions. This was explained by the presence of coeluting Gb3 subclasses (the ceramide moiety CM being either saturated, mono-unsaturated fatty acyl with a slightly higher migration distance, or polar hydroxyl fatty acyl with the opposite effect on migration) and of coeluting Gb3 isoforms (the hexoside moiety consisting of glucose and/or galactose units). This resulted in the broadening and partial splitting of the standard band. In the plasma samples, 19 molecular species of Gb3 were identified (depending on the CM, the sugar isoforms being undistinguishable by MS): 5 with a saturated CM, 7 with two additional double bonds on the CM, 7 with a methylated CM. In case of Fabry’s disease, most Gb3 species with saturated CM were highly increased, whereas other species were decreased.

      Classification: 4e, 11c, 11e, 32f
      130 004
      Identification of acetylcholinesterase inhibitors in water by combining two-dimensional thin-layer chromatography and high-resolution mass spectrometry
      Lena STÜTZ*, W. SCHULZ, R. WINZENBACHER (*Laboratory for Operation Control and Research, Zweckverband Landeswasserversorgung, Langenau, Germany; stuetz.l@lw-online.de)

      J Chromatogr A, 1624, 461239 (2020). Samples were chemical standards of acetylcholinesterase (AChE) inhibitors (azamethiphos, caffeine, donepezil, galanthamine, methiocarb-sulfoxide, paraoxon-ethyl) and of neurotoxic compounds, as well as drinking or contaminated water samples enriched through solid phase extraction. HPTLC on spherical silica gel (pre-washed twice by 20 min immersion in isopropanol, heated 20 min at 120 °C before and after pre-washing with acetonitrile). First separation (preparative TLC) with automated multiple development (16 steps). Effect-directed analysis for AChE inhibitors by immersion (speed 5 cm/s, time 1 s) into enzyme solution, incubation 5 min at 37 °C and immersion into substrate solution (indoxyl acetate 2 % in methanol); visualization under UV 366 nm. Active zones from untreated layers were eluted through the oval head of a TLC-MS interface to a second plate for a second separation with a panel of other mobile phases. Bands of interest were eluted from the second layer with water through the oval elution head of the TLC-MS interface pump, into a RP18 liquid chromatography guard column, followed by a quadrupole time-of-flight mass spectrometer. Full scan mass spectra (m/z 100–1200) were recorded in negative and positive modes using electrospray ionization (and collision-induced dissociation for MS2). Among the water contaminants, lumichrome (riboflavin photolysis product), paraxanthine and linear alkylbenzene sulfonates were identified as AChE inhibitors.

      Classification: 3d, 4d, 4e, 22, 29b, 35d, 37c
      130 007
      Planar chromatography-bioassays for the parallel and sensitive detection of androgenicity, anti-androgenicity and cytotoxicity
      C. RIEGRAF, A.M. BELL, M. OHLIG, G. REIFFERSCHEID, S. BUCHINGER* (*Federal Institute of Hydrology, Koblenz, Germany; buchinger@bafg.de)

      J Chromatogr A, 1684, 463582 (2022). Samples were concentrated filtrates of leachates of waste deposition sites, as well as testosterone, flutamide, bisphenol A (BPA) and nitroquinoline oxide (NQO) as standards. Automated Multiple Development on HPTLC silica gel (prewashed with methanol and dried 30 min at 110 °C) with 1) methanol up to 20 mm; 2A) chloroform – ethyl acetate –petroleum ether 11:4:5 or 2B) ethyl acetate – n-hexane 1:1 for flutamide and testosterone, up to 90 mm. Effect-directed analysis was performed by automated spraying 3 mL suspension of BJ1991 yeast (transfected Saccharomyces cerevisiae strain, pure for androgenic activity, with 50 ng/mL testosterone for anti-androgenic assay), followed by 20 h incubation at 30 °C in a closed chamber (90 % relative humidity), by 5 min drying under cold air stream, by spraying 2.5 mL MUG solution (4-methylumbelliferyl-galactopyranoside) and by 15 min incubation at 37 °C in an open chamber. Agonistic and antagonistic activities were detected qualitatively under UV 366 nm (light or dark blue bands, respectively, on blue background) and quantitatively documented using automated scanning at excitation wavelength 320 nm (deuterium lamp), with cut-off filter at 400 nm. Dose-response curves for model compounds were established by regression analysis. Anti-androgenic effective doses at 10 % were 28 ng/zone for flutamide and 20 ng/zone for BPA, without toxicity for the yeast. To exclude cytotoxicity where anti-androgenic activity was observed, the HPTLC layers (either without or after the spraying with MUG) were sprayed with 3 mL resazurin solution (0.01 % in water) and incubated 30 min at 30 °C and 90 % humidity. Cytotoxicity bands appeared as pink zones of resorufin on a colorless background (dihydroresorufin) under white light. Densitometric evaluation in absorption mode at 575 nm (under deuterium and halogen-tungsten lamps, no filter applied). NQO was cytotoxic at its lowest tested dose (1 ng/zone).

      Classification: 4b, 4e, 32d, 37c, 37d
      128 035
      The bacterial microbiome of the long-term aquarium cultured high microbial abundance sponge Haliclona cnidata – sustained bioactivity despite community shifts under detrimental conditions
      J. SCHELLENBERG, J. REICHERT, M. HARDT, I. KLINGELHÖFER, G. MORLOCK, P. SCHUBERT, M. BIŽIĆ, H.-P. GROSSART, P. KÄMPFER, T. WILKE, Stefanie P. GLAESER* (*Research Centre for BioSystems, Land Use and Nutrition, Institute of Applied Microbiology, Justus Liebig University Giessen, Giessen, Germany; stefanie.glaeser@umwelt.uni-giessen.de)

      Frontiers in Marine Science 7, 266 (2020). Methanol extracts from marine sponge Haliclona cnidata (Chalinidae) submitted to different stresses (antibiotics and/or darkness) were separated on HPTLC silica gel with an automated 15-step gradient based on methanol, dichloromethane and n-hexane. Bioluminescence was recorded after immersing the HPTLC plates into Aliivibrio fischeri suspension. Antibacterial activity and quorum sensing enhancement were analysed on software, and Pearson’s similarity coefficient was applied to generate similarity matrices for cluster analysis (UPGMA, Unweighted Pair Group Method with Arithmetic Mean). Only slight differences were observed, especially in QS enhanced zones in stressed vs. control cultures.

       

      Classification: 32e
      128 092
      Honeybee colonies compensate for pesticide-induced effects on royal jelly composition and brood survival with increased brood production
      M. SCHOTT, M. SANDMANN, J.E. CRESSWELL, M.A. BECHER, G. EICHNER, D.T. BRANDT, R. HALITSCHKE, S. KRUEGER, G. MORLOCK, R.-A. DÜRING, A. VILCINSKAS, M.D. MEIXNER, R. BÜCHLER, Annely BRANDT* (*LLH Bee Institute, Landesbetrieb Landwirtschaft Hessen, Kirchhain, Germany; annely.brandt@llh.hessen.de)

      Nature - Sci. Rep. 11, 62 (2021). Samples were isopropylacetate – methanol 3:2 fractions of (1) n-hexane extracts of larvae of Apis mellifica carnica (Apidae) from hives exposed to different concentrations of neonicotinoid pesticide clothianidin in their food, as well as (2) worker jelly adsorbed from brood combs of the same hives on adsorptive filter strips (unused filter strip parts were kept as background control). HPTLC on silica gel with chloroform – methanol – water – ammonia 30:17:2:1 for (1), and with an 8-step gradient based on methanol, chloroform, toluene, and n-hexane for (2, see CBS 105: Optimization of an AMD 2 method for determination of stratum corneum lipids). Visualization at UV 366 nm before and after derivatization by immersion into primuline reagent (primuline 0.5 g/L in acetone – water 4:1). Furthermore, antibacterial activity of (2) was assessed by recording the bioluminescence on the HPTLC plates, neutralized after elution and immersed into Aliivibrio fischeri suspension. Semi-quantitative comparison showed that a higher exposure to clothianidin was correlated with a decrease in lipid composition as well as in antibacterial activity.

      Classification: 11, 37
      115 024
      Quantitative errors and uncertainty in high-performance thin-layer chromatography method for quality assessment of Calendula officinalis plant extracts
      Snezana AGATONOVIC-KUSTRIN*, Christine LOESCHER, D. MORTON (*School of Pharmacy and Applied Science, La Trobe Institute of Molecular Sciences, La Trobe University, Bendigo, Australia, s.kustrin@latrobe.edu.au)

      J. Planar Chromatogr. 28, 213-217 (2015). HPTLC of (1) chlorogenic acid, (2) caffeic acid, (3) faradiol and (4) rutin from Calendula officinalis plant extracts on silica gel previously activated at 50 °C in an oven for 30 min. Automated multiple development (gradient elution) with n-hexane, ethyl acetate containing 2 % acetic acid, and water as mobile phase. Detection by spraying with either 10 % sulfuric acid in methanol or 2-aminoethyl diphenylborinate solution followed by placing in oven at 50 °C for 30 min. (1), (2), (3), and (4) were used as markers to investigate and assess the quantitative errors observed. Accuracy of the sample applicator at different sample volumes, the use of a gradient mobile phase, and post-derivatization contribute to uncertainties of the HPTLC method and need to be carefully selected to minimize errors.

      Classification: 2f, 8a, 32e
      68 148
      Application of AMD to the determination of crop protection agents in drinking water
      K. BURGER, J. KÖHLER, H. JORK*, (*Univ. des Saarlandes, Fachber. Pharm. und Biol. Chem., D-W-6600 Saarbrücken, FRG)

      J. Planar Chromatogr. 3, 504-510 (1990). Multiple and stepwise development combined with gradient elution as a highly suitable method for the systematic determination of crop protection agents. The migration distance is highly reproducible (on the same HPTLC plate and on different ones). Screening and confirmation gradients coupled with reflectance spectroscopy (multiwavelength scanning) and postchromatographic, microchemical derivatization make it possible to detect crop protection agents in drinking, table, and ground waters. At least 100 substances can be checked for their presence on one HPTLC plate. Example: HPTLC separation of 21 crop protection agents in ground and drinking water with AMD. Two 23-step gradients (33 runs) based on acetonitrile, dichloromethane, hexane, formic acid, NH3 25% and on tert buthyl methyl ether, acetonitrile, hexane, formic acid, NH3. Multiwavelength scanning by adsorbance at 190, 220, 240, 260, 280, and 300 nm

      Classification: 29
      72 027
      Use of linear solvent gradients in manual and automated multiple development for the separation and characterization of drugs and metabolites by HPTLC
      P.V. COLTHUP, J.A. BELL, D.L. GADSDON, (Drug Metabolism Div., Glaxo Group Res. Ltd., Park Road, Are, Herts, SG12 ODP, UK)

      J. Planar Chromatogr. 6, 386-393 (1993). Novel solvent gradient, with a linear eluotropic strength profile, comprising binary solvent mixtures from methanol to hexane. The chromatographic behavior of 55 compounds selected as models from phase I and phase II drug metabolism transformation has been studied using this linear solvent gradient with both manual and automated multiple development. The data obtained demonstrate the potential of HPTLC with linear solvent gradients for the separation and characterization of drugs and metabolites.

      Classification: 3d