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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      129 055
      Elicitation of antioxidant metabolites in Musa species in vitro shoot culture using sugar, temperature and jasmonic acid
      I.O. AYOOLA-ORESANYA, B. GUEYE, M.A. SONIBARE, M.T. ABBERTON, Gertrud E. MORLOCK* (*Institute of Nutritional Science, Justus Liebig University Giessen, and TransMIT Center of Effect-Directed Analysis, Giessen, Germany; gertrud.morlock@uni-giessen.de)

      Plant Cell, Tissue and Organ Culture (PCTOC) 146 (2), 225–236 (2021). Samples were hydro-ethanolic extracts of Musa acuminata and M. balbisiana (Musaceae) plantlets, obtained from in vitro meristem-derived gel cultures with saccharose, temperature or jasmonic acid as elicitors of production of secondary metabolites. HPTLC on silica gel  (RP18W phase for genotoxicity assay) with ethyl acetate – toluene – formic acid – water 34:5:7:5. Evaluation under white light, UV 254 nm and 366 nm. Effect-directed assays (EDA) were performed (by immersion or by automated piezoelectrical spraying) for free radical (DPPH•) scavengers, and, after neutralization, for enzymatic inhibitors (acetyl-cholinesterase, α-glucosidase) and for genotoxicity (SOS response – UMU-C test). For comparison, positive control standards were applied but not developed, before the assays (gallic acid, physostigmine, acarbose, nitroquinoline-1-oxide, respectively). After the first assay, absorbance densitometry was performed through inverse scanning at 546 nm using mercury lamp (fluorescence mode without optical filter). Antioxidant activity was found the highest when cultures were maintained at 20 °C (vs. 15 and 26 °C) and supplemented with saccharose (40-50 g/L) or jasmonic acid (200 µM).

      Classification: 4e, 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; gertrud.morlock@uni-giessen.de)

      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
      129 068
      Thai mango and pineapple puree and juice analyzed by high-performance thin-layer chromatography hyphenated with effect-directed assays
      Gertrud E. MORLOCK*, N. WUTTHINITHISANAND, D. RAUHUT
      (*Institute of Nutritional Science, and Interdisciplinary Research Centre for Biosystems, Land Use and Nutrition, Justus Liebig University Giessen, Giessen, Germany; gertrud.morlock@uni-giessen.de)

      Molecules, 26 (24), 7683 (2021). Samples were ultrasound-assisted extracts of fruit puree and juice (pre-treated with sulfur dioxide or ascorbic acid) of Ananas comosus (Bromeliaceae) and Mangifera indica (Anacardiaceae). HPTLC on silica gel with toluene – ethyl acetate – methanol – formic acid 120:90:35:3. Detection under white light, UV 254 nm and 366 nm, before and after  derivatization by immersion (2 s, 3 cm/s) into anisaldehyde sulfuric acid reagent and  diphenylamine aniline reagent, followed by heating at 110 °C for 5 min. Effect-directed analysis using automated immersion: A) for free radical (DPPH•) scavengers; B) for enzymatic inhibition (acetyl-cholinesterase, tyrosinase); C) for activity against Gram-negative (Aliivibrio fischeri bioluminescence assay) or Gram-positive bacteria (Bacillus subtilis bioassay). Active compounds were far more present in puree than in juice extracts, and differences were also seen between cultivars. Ascorbic acid (hRF 37), used as additive for the mango puree, was active as antioxidant and as transiently disruptive for A. fischeri metabolism and bioluminescence.

      Classification: 27, 32e, 35b
      129 065
      Effect-directed analysis of bioactive compounds in Cannabis sativa L. by high-performance thin-layer chromatography
      G. CORNI, V. BRIGHENTI, F. PELLATI, Gertrud E. MORLOCK*
      (*Institute of Nutritional Science, Justus Liebig University Giessen, and TransMIT Center of Effect-Directed Analysis, Giessen, Germany; gertrud.morlock@uni-giessen.de)

      J Chromatogr A, 1629, 461511 (2020). HPTLC of methanolic extracts of female inflorescences from ten hemp varieties (Cannabis sativa, Cannabaceae) on silica gel with toluene – ethyl acetate 1:1 or (for yeast assays) on RP-18W with toluene – ethyl acetate 7:3. 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. Chromatograms were documented under white light, UV 254 nm and for fluorescence detection (FLD) at 366 nm. Afterwards, 6 derivatization assays were performed with the following reagents, either without heating: primuline; or requiring heating 5 min at 120 °C: p-aminobenzoic acid; anisaldehyde sulfuric acid; diphenylamine aniline phosphoric acid; ninhydrin; vanillin sulfuric acid. Besides, 8 effect-directed assays (EDA) were performed for free radical (DPPH•) scavengers, for antimicrobial compounds (Gram-positive Bacillus subtilis assay, Gram-negative Aliivibrio fischeri bioluminescence assay), for phytoestrogens (planar yeast estrogen assay), for inhibitors of the following enzymes: acetyl-cholinesterase (AChE), α- and β-glucosidase, tyrosinase. AChE assay was performed by immersion (speed 3.5 cm/s, time 5 s) into AChE solution (666 units in TRIS buffer 0.05 M, with bovine serum albumin 0.1 %, pH 7.8), incubation 25 min at 37 °C, spraying with substrate solution, and heating 2 min at 50 °C. Two AChE substrate solutions were used: A) α-naphthyl acetate 0.1 % and chromogenic reagent Fast Blue salt B 0.18 % in ethanol – water 1:2, giving white inhibition bands visible on purple background under white light; B) with 3-indoxyl-3-acetate, giving black inhibition bands on blue background under UV 254 nm, which was useful to prevent false negatives when Fast Blue Salt B formed colored bands with analytes. Two bands of multipotent compounds were eluted from normal-phase layer 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 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 and standards, they were identified as cannabidivarinic acid (hRF 55) and cannabidiolic acid (hRF 60-70).

      Classification: 4e, 7, 15a, 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; gertrud.morlock@uni-giessen.de)

      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
      128 089
      Effect-directed profiling of 32 vanilla products, characterization of multi-potent compounds and quantification of vanillin and ethylvanillin
      Gertrud E. MORLOCK*, M. BUSSO, S. TOMEBA, A. SIGHICELLI (*Institute of Nutritional Science, and TransMIT Center for Effect-Directed Analysis, Justus Liebig University Giessen, Giessen, Germany; gertrud.morlock@uni-giessen.de)

      J Chromatogr. A, 1652, 462377 (2021). Samples were vanilla tinctures, water − ethanol − ethyl acetate 1:1:1 extracts of vanilla-flavored food products and of natural Vanilla sp. (Orchidaceae) pods, oleoresin, paste and powders, as well as calibration standards of vanillin (1) and ethylvanillin (2). HPTLC on silica gel with n-hexane – ethyl acetate 1:1 for profiling, 3:2 for quantification. Other mobile phases were also tested and given in the supplement. Compounds (1) and (2) (hRF 68 and 82, respectively) were quantified by absorbance densitometry (at maximal wavelength 310 nm, deuterium lamp, scanning speed 10mm/s). Contents were found to be between 1 μg/g and 36 mg/g for (1) and null for (2) except in one tincture (62 µg/mL). Derivatizations performed for five assays: A) to detect radical scavengers, immersion (speed 3 cm/s, time 5 s) into DPPH• (0.5 mM in methanol), followed by drying for 90 s at room temperature and 30 s at 60 °C; B) to detect activity against Gram-negative bacteria, immersion (speed 2 cm/s, time 3 s) into Aliivibrio fischeri suspension, followed by recording the bioluminescence; C) to detect activity against Gram-positive bacteria, immersion (speed 3.5 cm/s, time 6 s) into Bacillus subtilis, followed by incubation 2 h at 37 °C, immersion in MTT solution, incubation for 30 min at 37 °C and heating for 5 min at 50 °C; D) to detect acetylcholinesterase (AChE) inhibitors, immersion (speed 2.5 cm/s, time 2 s) into AChE solution (666 units in TRIS buffer 0.05M, with bovine serum albumin 0.1 %, pH 7.8), incubation for 25 min at 37 °C and immersion into substrate solution (α-naphthyl acetate 0.1 % and Fast Blue salt B 0.18 % in ethanol – water, 1:2; E) to detect tyrosinase inhibitors, spraying with enzyme solution (400 unit/mL, in phosphate buffer 0.02 M, pH 6.8), followed by 2 min drying, immersion into substrate levodopa (18 mM in phosphate buffer, pH 6.8), 10 min incubation at room temperature and drying. For identification, zones of interest were transferred with methanol from underivatized HPTLC layer through a TLC-MS interface and a filter frit directly to a Quadrupole-Orbitrap MS (heated electrospray ionization, probe heater at 270°C, spray voltage 3.5kV, lock masses acetic acid for negative, dibutyl phthalate for positive ionization, mode full HR-MS scan in m/z range 50–750). Afterwards, the following substances assigned by MS were confirmed by using HPTLC comparison with standards: (1) and (2), vanillyl alcohol, vanillic acid, ethyl vanillyl ether, coumarin, 4-hydroxybenzoic acid, 4-methoxybenzoic acid, 4-hydroxybenzaldehyde, 4-allyl benzoic acid, oleamide, triacetin.

      Classification: 4e, 7, 8b, 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
      127 032
      Identification and quantification of cannabinol as a biomarker for local hemp retting in an ancient sedimentary record by HPTLC-ESI-MS
      T. SCHMIDT, Annemarie KRAMELL*, F. OEHLER, R. KLUGE, D. DEMSKE, P. TARASOV, R. CSUK (*Department of Organic Chemistry, Martin-Luther-University Halle-Wittenberg, Kurt-Mothes-Str. 2, 06120 Halle, Germany, annemarie.kramell@chemie.uni-halle.de)

      Anal. Bioanal. Chem. 412, 2633-2644 (2020). HPTLC of  cannabinol in sediment samples on silica gel with n-heptane - diethyl ether 9:1. Detection by spraying with cerium- molybdenum reagent (400 mg cerium IV sulfate and 20 g ammonium molybdate in 400 mL 10 % sulfuric acid). HPTLC plates were further analyzed by electrospray ionization mass spectrometry. The hRF value for cannabinol was 20. Linearity was between 25 and 155 ng/zone. Intermediate precision was below 5 % (n=3). The LOD and LOQ were 6 and 21 ng/zone. Average recovery was 73 %.

      Classification: 8b