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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      130 004
      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;

      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
      130 006
      Thin-layer chromatography with eutectic mobile phases – preliminary results
      Danuta RAJ* (*Department of Pharmacognosy and Herbal Medicines, Wroclaw Medical University, Wroclaw, Poland;

      J Chromatogr A, 1621, 461044 (2020). Samples were five isoquinoline alkaloids (berberine, chelerythrine, chelidonine, coptisine, sanguinarine) either as standard mixture or present in a Chelidonium majus (Papaveraceae) herb extract obtained with HCl 0.05 M in methanol. Separation on TLC and HPTLC silica gel layers with a screening of mobile phases consisting of eutectic mixtures of chemicals and/or phytochemicals. These homogenous stable liquids called DES (deep eutectic solvents) were obtained either simply by mixing, or by mixing followed by heating at 50°C, or by mixing with water for dissolution followed by dehydratation through rotary evaporation. For polarity adjustment, the DES phases were tested pure or diluted with acetone, chloroform, diethyl ether, methanol, or water. Visualization under UV 366 nm. The best separation was obtained with menthol – phenol in equimolar mixture, with 35 % methanol added (hRF values of the selected alkaloids were 33, 39, 79, 20 and 52, respectively).

      Classification: 22, 32e
      129 061
      Effect-directed profiling of powdered tea extracts for catechins, theaflavins, flavonols and caffeine
      (*Institute of Nutritional Science, Justus Liebig University Giessen, and TransMIT Center of Effect-Directed Analysis, Giessen, Germany;

      Antioxidants, 10(1), 117 (2019). Samples were methanolic extracts of Camellia sinensis leaves or commercial black, white or green tea powdered extracts (Theaceae), as well as standards of caffeine (methylxanthine alkaloid), of flavonols (quercetin, rutin) and of flavanols (catechin, catechin-gallate, epicatechin, epicatechin-gallat, epigallocatechin, epigallocatechin-gallate, gallocatechin, and the thearubigin theaflavin). HPTLC on RP18-W phase (with classical irregular particles (SP1) vs. LiChrospher phase with spherical particles (SP2)), prewashed with methanol – water 4:1 and dried 20 min at 110 °C, developed with citric acid 0,295 % in acetonitrile – water 3:10 for SP1, with citric acid 0,17 % in acetonitrile – water 1:2 for SP2. Visualization under white light, UV 254 nm and 366 nm. Absorbance densitometry was performed at UV 275 nm (deuterium lamp). Derivatization with A) Fast Blue B salt reagent followed by 3 min heating at 100 °C, and by absorbance densitometry at 546 nm for flavanols (mercury lamp); B) natural product reagent (on the same plate), followed by fluorescence densitometry of flavonols at FLD 366/>400 nm (mercury lamp); C) anisaldehyde sulfuric acid reagent, followed by 2 min heating at 110 °C, to detect all flavonoids. Effect-directed analysis was performed using piezoelectric spraying: A) for free radical (DPPH•) scavengers (vs. gallic acid as positive control); B) for activity against Gram-negative Aliivibrio fischeri (bioluminescence assay, vs. caffeine) or Gram-positive Bacillus subtilis (vs. tetracycline); C) for enzymatic inhibition of acetyl-cholinesterase, α- and β-glucosidase, β-glucuronidase, tyrosinase (vs. rivastigmine, acarbose, imidazole, D–saccharolactone and kojic acid, respectively). When SP2 was used, previous neutralization was required through spraying of sodium bicarbonate buffer (2.5 %, pH 8). AChE inhibition assay was performed with indoxyl acetate (0.1 % in ethanol) as substrate, sprayed before the enzyme. After incubation (30min at 37°C), inhibition bands appeared indigo or blue under white light, but the substrate coloured theaflavin in yellow.

      Classification: 4e, 8a, 22, 32e
      129 063
      Automated piezoelectric spraying of biological and enzymatic assays for effect-directed analysis of planar chromatograms
      E. AZADNIYA, Gertrud E. MORLOCK* (*Institute of Nutritional Science, Justus Liebig University Giessen, and TransMIT Center of Effect-Directed Analysis, Giessen, Germany;

      J Chromatogr A, 1602, 458–466 (2019). HPTLC of caffeine, physostigmine (alkaloids) and hydroethanolic extract of Peganum harmala seeds (Nitrariaceae, Zygophyllaceae) on silica gel prewashed twice with methanol – water 3:1, followed by 1 h drying at 120 °C. Separation, after 5 min chamber saturation, with ethyl acetate – methanol – ammonia (25%) 85:11:4 (basic mobile phase) or ethyl acetate – toluene – formic acid – water 16:4:3:2 (acidic mobile phase, requiring neutralization with phosphate-citrate buffer). Derivatization with Dragendorff’s reagent and with anisaldehyde sulfuric acid. Effect-directed analysis by spraying A) with Gram-negative bioluminescent Aliivibrio fischeri suspension for antibacterial activity (caffeine was used as standard); B) with acetyl- and butyryl-cholinesterase (AChE / BChE) solutions for enzymatic inhibition. For AChE and BChE asssays, classical immersion into the enzyme solutions was also used for comparison, and inhibition densitometry for active analytes was performed by inverse scan measurement (fluorescence without optical filter) at 546 nm using a mercury lamp; activity was expressed as physostigmine equivalents. Active bands were eluted (only after basic MP) with methanol through the oval elution head of a TLC-MS interface pump, into a quadrupole-Orbitrap mass spectrometer. Full scan mass spectra (m/z 50−750) in positive ionization mode were recorded using heated electrospray ionization (HESI, spray voltage 3.5kV, capillary temperature 270°C). By comparison to literature, AChE inhibitors (also active against A. fischeri) were assigned to be harmine, harmaline and ruine (β-carboline alkaloids), and BChE inhibitors were harmol (same class) and vasicine and deoxyvasicine (quinazoline alkaloids, also called peganine and deoxypeganine). Piezoelectric spraying had the following advantages over automated immersion: (1) it covered the whole plate surface; (2) required much lower volumes of solutions; (3) applied always fresh enzyme or reagent solutions, thus avoiding gradual inactivation; (4) avoided zone distortions, shifts or tailings occurring during immersion or withdrawal of the plate, or due to the hydrophilicity of compounds.

      Classification: 3e, 4e, 22, 32e
      129 066
      Effect-directed profiling of 17 different fortified plant extracts by high-performance thin-layer chromatography combined with six planar assays and high-resolution mass spectrometry
      Gertrud E. MORLOCK*, J. HEIL, V. BARDOT, L. LENOIR, C. COTTE, M. DUBOURDEAUX (*Institute of Nutritional Science, Justus Liebig University Giessen, and TransMIT Center of Effect-Directed Analysis, Giessen, Germany;

      Molecules, 26 (5), 1468 (2021). Summary: Samples were fortified extracts produced with iPowder technology (involving spray-drying of a rich first extract on a new batch of the same plant) from following plants: Camellia sinensis final bud and two leaves (Theaceae), Cynara scolumus leaves and Echinacea purpurea roots (Asteraceae), Eleutherococcus senticosus roots (Araliaceae), Equisetum arvense aerial part (Equisetaceae), Eschscholzia californica aerial parts (Papaveraceae), Humulus lupulus cones (Cannabaceae), Ilex paraguariensis leaves (Aquifoliaceae), Melissa officinalis aerial parts and Rosmarinus officinalis leaves (Lamiaceae), Passiflora incarnata aerial part (Passifloraceae), Raphanus sativus var. niger roots (Brassicaceae), Ribes nigrum leaves (Grossulariaceae), Spiraea ulmaria floral tops (Rosaceae), Valeriana officinalis roots (Caprifoliaceae), Vitis vinifera leaves or pomace (Vitaceae). HPTLC on silica gel with 1) ethyl acetate – toluene – formic acid – water 16:4:3:2,  or 2) cyclohexane – ethyl acetate – formic acid 30:19:1. Detection under white light, UV 254 nm and 366 nm. Extract stability after 2 years was also checked through HPTLC. Neutralization by spraying phosphate-citrate buffer, and drying in cold air stream. Effect-directed analysis using automated piezoelectrical spraying: A) for enzymatic inhibition (acetyl-cholinesterase, glucosidase, glucuronidase, tyrosinase); B) for activity against Gram-negative bacteria (Aliivibrio fischeri bioluminescence assay). Active bands of multipotent compounds were eluted from HPTLC layers with methanol through the oval elution head of a TLC-MS interface pump, into a quadrupole-Orbitrap mass spectrometer. Full scan mass spectra (m/z 100−1000) in the positive and negative ionization modes were recorded using heated electrospray ionization (HESI, spray voltage 3.5 kV, capillary temperature 270 °C). By comparison to literature, the following compounds were assigned: caffeine, catechins, carnosol, chlorogenic acid, cynaratriol, dicaffeoylquinic acid, feruloyl quinic acid, gallic acid, linoleic and linolenic acids, oleanic or ursolic acid, rosmarinic acid.

      Classification: 4e, 7, 8a, 8b, 11a, 15a, 22, 32e
      129 064
      Effect-directed profiling and identification of bioactive metabolites from field, in vitro-grown and acclimatized Musa spp. accessions using high-performance thin-layer chromatography-mass spectrometry
      I.O. AYOOLA-ORESANYA, M.A. SONIBAREA, B. GUEYEB, R. PALIWALB, M.T. ABBERTON, Gertrud E. MORLOCK* (*Institute of Nutritional Science, and Interdisciplinary Research Centre for Biosystems, Land Use and Nutrition, Justus Liebig University Giessen, Giessen, Germany;

      J Chromatogr A, 1616, 460774 (2020). Methanolic extracts of leaves of Musa acuminata, M. balbisiana and M. sapientum (Musaceae), either from fields or from in vitro cultures or from the plantlets derived from in vitro culture and acclimatized in isolated warm room, were separated on HPTLC silica gel layers with toluene – ethyl acetate – methanol 6:3:1 or ethyl acetate – toluene – formic acid – water 34:5:7:5. When intended for MS experiments, layers were previously washed twice with methanol – formic acid 10:1, once with acetonitrile – methanol 2:1 and air-dried. Evaluation under white light, UV 254 nm and 366 nm. Derivatization by immersion (2s, 2cm/s) into natural product reagent preceded by heating at 110 °C for 5 min, or into anisaldehyde sulfuric acid reagent, diphenylamine aniline reagent, ninhydrin reagent, followed by the same heating procedure. Besides, plates were neutralized by cold air stream followed with phosphate buffer (8 %, pH 7.5) piezoelectrically sprayed on the plates and automated plate drying. Thereafter, 9 effect-directed assays (EDA) were performed for free radical (DPPH•) scavengers, for enzymatic inhibitors (α-amylase, acetyl- and butyryl-cholinesterase, α- and β-glucosidase), for antimicrobial compounds (Gram-positive Bacillus subtilis assay, Gram-negative Aliivibrio fischeri bioluminescence assay), and for mutagenic compounds (SOS response – UMU-C test using Salmonella typhimurium suspension and 4-nitroquinoline 1-oxide as positive control). The bands of 4 active compounds were eluted with methanol through a TLC-MS interface pump into a quadrupole-Orbitrap mass spectrometer. Full scan mass spectra (m/z 50−800) in the positive and negative ionization modes were recorded using electrospray ionization (ESI, spray voltage 3.3kV, capillary temperature 320°C, collision energy 35 eV). By comparison to a standard, one band present in all samples was identified as linolenic acid. For the other bands, only present in in vitro grown accessions, only raw molecular formulas and phytochemical classes were assigned (a pyrrolidine alkaloid, an amino-acid, a phenolic derivative).

      Classification: 4e, 7, 11a, 18a, 22, 32e
      129 052
      Herbal standardization of formulation containing curcuminoids, piperine and ascorbic acid by dual detection mode densitometric analysis
      P. PATEL*, J. BHATT, F. SUREJA, M. DHORU, K. DETHOLIA (*Department of Pharmaceutical Quality Assurance, Smt. S.M. Shah Pharmacy College, Mahemdabad, Gujarat, India,

      J. Planar Chromatogr. 34, 513-520 (2021). HPTLC of curcumin (1), piperine (2) and ascorbic acid (3) in a combined marketed formulation on silica gel with chloroform - methanol - ether - glacial acetic acid 95:3:1:1. Quantitative determination by absorbance measurement at 254 nm for (3) and in fluorescence mode at 366 nm for (1) and (2). The hRF values for (1) to (3) were 65, 83 and 28, respectively. Linearity was between 620 and 3040 ng/zone for (1), 470 and 2380 ng/zone for (2) and 530 and 2670 ng/zone for (3). Interday and intra-day precisions were below 2 % (n=3). 

      Classification: 22, 27
      129 049
      Quantification of piperine in different varieties of Piper nigrum by a validated high‑performance thin‑layer chromatography‒ densitometry method
      S. JANA, D. SING, S. BANERJEE, P. HALDAR, B. DASGUPTA, A. KAR, N. SHARMA, R. BANDYOPADHAYAY, P. MUKHERJEE (*Department of Pharmaceutical Technology, School of Natural Product Studies, Jadavpur University, Kolkata 700032, India,

      J. Planar Chromatogr. 34, 521-530 (2021). HPTLC of piperine in Piper nigrum on silica gel with toluene - ethyl acetate 3:2. Quantitative determination by absorbance measurement at 254 nm. The hRF value for piperine was 63. Linearity was between 200 and 1000 ng/zone. Interday and intra-day precisions were below 1 % (n=3). The LOD and LOQ were 611 and 1778 ng/zone, respectively. Average recovery was 98.3 %.

      Classification: 22