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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      130 001
      Separation and detection of apricot leaf triterpenes by high-performance thin-layer chromatography combined with direct bioautography and mass spectrometry
      Ágnes M. MÓRICZ*, P. G. OTT (*Plant Protection Institute, Centre for Agricultural Research, 1022 Budapest, Hungary; moricz.agnes@agrar.mta.hu)

      J Chromatogr A, 1675, 463167 (2022). Samples were ethanol extracts (and their flash chromatography fractions) of Prunus armeniaca leaves (Rosaceae), as well as betulinic, linolenic, maslinic (= crataegolic), oleanolic, ursolic acids and pygenic acids A (= corosolic acid) and B b as standards. When needed, to improve separation of triterpenoids, reversible pre-chromatographic derivatization was performed in situ by applying 10 µL iodine solution (2 % in chloroform) either before development on the deposit band, or for 2D-HPTLC after a first separation up to 60 mm and before a second orthogonal separation. Layers were covered 10 min with glass sheet after iodine application, and then dried 1 min under cold air stream. HPTLC on silica gel with chloroform – ethyl acetate – methanol 20:3:2, 85:9:6, or 15:2:3), followed by 5-10 min drying under cold air stream (eliminating iodine completely). Post-chromatographic derivatization by immersion (time 2 s, speed 3 cm/s) into vanillin – sulfuric acid (40 mg and 200µL, respectively, in 10 mL ethanol), followed by heating 5 min at 110 °C. Antibacterial effect-directed analysis was performed by immersion (time 8 s) into Bacillus subtilis suspension, followed by 2 h incubation at 37 °C, immersion in MTT solution and 30 min incubation at 37 °C. Active bands were eluted from layer with methanol through the oval elution head of a TLC-MS interface pump, into a single quadrupole mass spectrometer to record full scan mass spectra (m/z 200–1200 in both modes) using electrospray ionization (interface temperature 350°C, heat block temperature 400°C, desolvation line temperature 250°C, detector voltage 4.5kV). Five triterpenoids were identified: betulinic, corosolic, maslinic, oleanolic and ursolic acids, acid, as well as two fatty acids: linolenic and palmitic acid.

      Classification: 4e, 11a, 15a, 32e
      129 062
      Effect-directed analysis by high-performance thin-layer chromatography for bioactive metabolites tracking in Primula veris flower and Primula boveana leaf extracts
      E. MAHRAN, I. ELGAMAL, M. KEUSGEN, 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, 1605, 460371 (2019). HPTLC of toluene – ethyl acetate extracts of Primula boveana leaves and of P. veris (Primulaceae) on silica gel with n-hexane – ethyl acetate 7:3. Visualization under white light, UV 254 nm and 366 nm. Derivatization by spraying with anisaldehyde sulfuric acid reagent, followed by heating for 4 min at 105 °C. Effect-directed analysis: A) for activity against Gram-negative (Aliivibrio fischeri bioluminescence assay) or Gram-positive bacteria (Bacillus subtilis bioassay) using automated immersion; B) for enzymatic inhibition (acetyl- and butyryl-cholinesterase) using piezoelectric spraying, with rivastigmine as standard, and absorbance spectra (500 nm) for P. boveana active bands measured by inverse scanning. Active bands were eluted from the untreated layer with methanol through the oval elution head of a TLC-MS interface pump, into a quadrupole-Orbitrap mass spectrometer to record full scan mass spectra (m/z 100−1000) using electrospray ionization (ESI voltage 3.5kV for P. boveana, -3kV for P. veris, source temperature 250°C). With the further help of preparative HPLC – NMR, they were identified as linoleic and linolenic acids in P. veris, and as flavone and its derivatives: hydroxyflavone, methoxyflavone and zapotin, in P. boveana.

      Classification: 4e, 8a, 11a, 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
      129 069
      Distinction and valorization of 30 root extracts of five goldenrod (Solidago) species
      Ágnes M. MÓRICZ*, M. JAMSHIDI-AIDJI, D. KRÜZSELYI, A. DARCSI, A. BÖSZÖRMÉNYI, P. CSONTOS, S. BÉNI, P.G.OTT, G.E. MORLOCK (*Plant Protection Institute, Centre for Agricultural Research, Hungarian Academy of Sciences, 1022 Budapest, Hungary; moricz.agnes@atk.hu)

      J Chromatogr A, 1611, 460602 (2020). Samples were methanolic root macerates of Euthamia graminifolia, Solidago canadensis, S. gigantea, S. rugosa and S. virgaurea (Asteraceae). HPTLC on silica gel with n-hexane – isopropyl acetate – acetone 16:3:1; or (for preparative TLC) on TLC silica gel with n-hexane – acetone 7:3, followed by scraping the layer and eluting with ethanol. When intended for MS experiments, layers were previously washed with methanol – water 4:1 and heated 20 min at 100 °C. Derivatization with vanillin – sulfuric acid reagent. Multivariate image analysis of the derivatized chromatograms allowed clear separation of samples according to species. Effect-directed analysis for: A) enzymatic inhibition by immersion into acetyl- and butyryl-cholinesterase, glucosidase and amylase solutions; B) activity against Gram-negative bacteria using Xanthomonas euvesicatoria chromogenic bioassay, and Aliivibrio fischeri and Pseudomonas syringae maculicola bioluminescence assays; C) activity against Gram-positive bacteria with Bacillus subtilis spizizenii bioassay. Two labdane diterpenes (solidagenone, hRF 47, and presolidagenone, hRF 55) in S. canadensis and two polyacetylenes (matricaria-esters = methyl-decadiene-diynoates, hRF 78 and 87 in HPTLC) in S. virgaurea were identified from multipotent zones by bioassay-guided purification through preparative TLC / HPLC, followed by HRMS and NMR, as well as by HPTLC hyphenated to quadrupole-orbitrap HRMS in 2 ways: A) by eluting with methanol the compounds from the plate through the oval elution head of a TLC-MS interface, with heated electro-spray ionization (HESI, spray voltage 3.5 kV, capillary temperature 270 °C, nitrogen as sheath and auxiliary gas, full scan in negative and positive ionization modes in m/z range 50-750); tandem mass spectra were acquired in parallel at fragmentation energy of 15-100 eV; B) without eluent with a DART interface (Direct Analysis in Real-Time, needle voltage 4 kV, grid voltage 50 V, helium as gas, temperature 500 °C, full scan in positive ionization mode in m/z range 100-750).

      Classification: 4d, 4e, 8b, 11a, 15a, 32e
      129 059
      Same analytical method for both (bio)assay and zone isolation to identify/quantify bioactive compounds by quantitative nuclear magnetic resonance spectroscopy
      E. AZADNIYA, L. GOLDONI, T. BANDIERA, 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, 1616, 461434 (2020). Samples were acetonic extracts of Malus domestica fruit peels (Rosaceae) and of Salvia officinalis, Thymus vulgaris and Origanum vulgare spice powders (Lamiaceae), as well as standards of maleic acid (dicarboxylic acid), carvacrol, thymol (phenolic monoterpenes), rosmanol (phenolic diterpene), betulinic acid, corosolic acid (CA), maslinic acid (MA), oleanolic acid (OA) and its isomer ursolic acid (UA) (triterpenes). HPTLC on silica gel, when intended for MS and NMR experiments, layers were prewashed twice with methanol – water 3:1, followed by 30 min drying at 120 °C. When intended for quantitative densitometry, start zones were submitted to prechromatographic derivatization with iodine solution (10 g/L in chloroform) allowed to migrate up to 12 mm, incubated 10 min at 27 °C and dried under cold air stream; this allowed separation of isomeric triterpenes. Separation with toluene – methanol – ethyl acetate 17:2:1 after 5 min chamber saturation at 50 % relative humidity. CA coeluted with MA, and OA with UA. Four hyphenations: A) Quantitative HPTLC densitometry for active analytes was performed by measuring absorption at 665 nm with a tungsten lamp after immersion of the chromatograms in anisaldehyde sulfuric acid reagent and heating 5 min at 110 °C. Linear range was obtained at 25 - 200 ng/band for OA and 100 - 400 ng/band for UA. B) Effect-directed analysis by immersing the chromatograms into Gram-positive Bacillus subtilis suspension for antibacterial activity and into acetyl-cholinesterase and tyrosinase solutions for enzymatic inhibition. C) Active bands were eluted with methanol through the oval elution head and in-line filter frit 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, probe heater temperature 200 °C). D) With higher amounts applied, preparative HPTLC, by scraping the multipotent band corresponding to OA and UA, and dissolving these analytes in methanol, for NMR analyses (1H raw or deconvoluted, and 2D 1H–13C Heteronuclear Single Quantum Coherence). Both isomers were distinguished by their allylic H-18 protons and separately quantified by applying PULCON method (PUlse Length-based CONcentration). LOQ was 267 μM for OA and 173 μM for UA; optimal range was 300 – 4600 mM, corresponding to 126 - 2090 μg of triterpenes.

      Classification: 4e, 7, 11a, 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
      129 058
      Effect-directed profiling of Ficus religiosa leaf extracts for multipotent compounds via 12 effect-directed assays
      V. GAWANDE, 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, 1637, 461836 (2021). Successive ultrasonic macerates of Ficus religiosa leaves (Moraceae) were separated with toluene – ethyl acetate – methanol 6:3:1 on HPTLC silica gel or (for yeast and genotoxicity assays) on RP18W phase. 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 366 nm. Afterwards, 11 derivatization assays were performed with the following reagents, either without heating: Dragendorff’s reagent; Fast Blue B salt; ferric chloride; natural product reagent - PEG 400; primuline; or requiring heating for 5 min at 120 °C: anisaldehyde sulfuric acid; diphenylamine aniline phosphoric acid; 2-naphthol sulfuric acid; ninhydrin; Tillmans' reagent; vanillin sulfuric acid. Besides, 12 effect-directed assays (EDA) were performed for free radical (DPPH• and ABTS•) scavengers, for enzyme inhibitors (α-amylase, acetyl- and butyryl-cholinesterase, α- and β-glucosidase, tyrosinase), for antimicrobial compounds (Gram-positive Bacillus subtilis assay, Gram-negative Aliivibrio fischeri bioluminescence assay), for phytoestrogens (planar yeast estrogen assay) and genotoxicity (SOS response – UMU-C test by successive immersions into citric buffer, into Salmonella typhimurium suspension and into methylumbelliferyl-galactopyranoside solution, followed by FLD at 366nm of mutagenic compounds as blue fluorescent zones, using 4-nitroquinoline 1-oxide as positive control). No activity was found for the last two assays. Ethyl acetate extracts of all samples were the most active. After EDA, most active bands were scanned for semi-quantitative equivalence densitometry at 546 nm using mercury lamp, compared to the following standards: acarbose, gallic acid, imidazole, kojic acid, physostigmine, tetracycline, depending on the assay. The bands of 3 multipotent compounds were eluted with methanol through the oval elution head and in-line filter frit 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 mode were recorded using heated electrospray ionization (HESI, spray voltage 3.5 kV, capillary temperature 270 °C, probe heater temperature 200 °C). MS-MS spectra were recorded in the negative mode using HCD-NCE (higher-energy collisional dissociation –normalized collision energy, with stepped negative collision energies from 10 to 40 eV). The three active zones were assigned to palmitic acid, to linolenic acid and to its di-oxygenated derivative.

      Classification: 4e, 11a, 32e
      129 019
      Rapid analytical approach for bioprofiling compounds with radical scavenging and antimicrobial activities from seaweeds
      P. RISTIVOJEVIC, V. JOVANOVIC, D. OPSENICA, J. PARK, Judith ROLLINGER, Tanja VELICKOVIC* (*University of Belgrade–Faculty of Chemistry, Studentski trg 12-16, 11158 Belgrade, Serbia, anja.velickovic@ghent.ac.kr)

      Food Chem. 334, 127562 (2021). HPTLC of five seaweed cultivars, namely three Saccharina japonica and two Undaria pinnatifida on silica gel with n-hexane - ethyl acetate - formic acid 30:50:1. Detection by spraying with anisaldehyde sulfuric acid reagent (1.5 mL of anisaldehyde was mixed with 210 mL of ethanol, 25 mL acetic acid and 13 mL conc. sulfuric acid), followed by heating at 120 °C for 3 min. Qualitative identification under UV light at 366 nm. HPTLC-bioautography antimicrobial assays by dipping into B. subtilis cell suspension, followed by incubation at 37 °C for 30 min and E. coli suspension, followed by incubation at 37 °C for 1 h. Visualization by dipping into a solution of MTT dye with triton X-100 (1 mg/mL). Stearidonic, eicosapentaenoic, and arachidonic acids were identified by HPLC-MS.

       

      Classification: 11c