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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      129 071
      Comparison of high-performance thin-layer with overpressured layer chromatography combined with direct analysis in real time mass spectrometry and direct bioautography for tansy root
      Ágnes M. MÓRICZ*, T.T. HÄBE, 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, 1603, 355–360 (2019). Samples were ethyl acetate root macerates of fully flowered Tanacetum vulgare (Asteraceae). HPTLC on silica gel (classical irregular particles vs. Lichrosphere with spherical particles) previously washed with methanol, dried for 5 min at room temperature, perimeter-sealed with a polymer coat, and heated for 30 min at 100 °C. Separation with toluene or with toluene – n-hexane 7:3, in classical capillary flow or in OPLC (overpressured layer chromatography). For OPLC, off-line infusion was used (closed mobile phase (MP) outlet, automatically stopping development); external pressure 50 bar, rapid MP flush 175 and 350 µL, MP flow rate 250 and 500 µL/min, 1830 and 3475 µL MP, development time 446 s and 424 s. Derivatization by immersion into vanillin – sulfuric acid reagent, followed by 5 min heating at 110 °C; or into PABA reagent (500 mg p-aminobenzoic acid, 18 mL glacial acetic acid diluted, 20 mL water, 1 mL o-phosphoric acid, 60 mL acetone), followed by 5 min heating at 140 °C. Effect-directed analysis using automated immersion: A) for free radical (DPPH•) scavengers; B) for activity against Gram-negative bacteria using Aliivibrio fischeri bioluminescence assay; C) for activity against Gram-positive bacteria with Bacillus subtilis bioassay. Four active polyynes were identified as hexadiynylidene-epoxy-dioxaspiro-decane (1), pontica epoxyde (nonene-triynyl-vinyl-oxirane) (2), tetradeca-triine-en-one (3) and trans-(hexadiynylidene)-dioxaspiro-decene (4), by hyphenating OPLC to quadrupole-orbitrap HRMS without eluent, using a DART interface (Direct Analysis in Real-Time, needle voltage 4kV, grid voltage 50 V, helium as gas, temperature 500 °C, full scan in positive ionization mode in m/z range 100-750). Polyynes (3) and (4) were coeluting in HPTLC but not in OPLC, demonstrating that (4) is not produced by oxidation during the DART-MS procedure. Separation with OPLC compared to HPTLC was performed in a shorter time and with better resolution at the same time. Layers with spherical particles gave higher resolution; zone distortions occurring in OPLC due to dissolved air in MP were prevented by previous MP sonication.

      Classification: 3b, 3d, 4e, 5a, 8b, 9, 32e
      129 070
      Effect-directed screening of Bacillus lipopeptide extracts via hyphenated high-performance thin-layer chromatography
      M. JAMSHIDI-AIDJI, I. DIMKIC, P. RISTIVOJEVIC, S. STANKOVIC, 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, 460366 (2019). Samples were standards and complex mixtures of non-ribosomally synthesized cyclic lipopeptides (CLPs) from Bacillus strains (Bacillaceae) found in soil or in manure: B. amyloliquefaciens (SS-12.6, SS-13.1, SS-27.2, SS-38.4) and B. pumilus (SS-10.7). Two extraction methods were compared: ethyl acetate extraction (Ex1), and the acidic precipitation followed by methanol extraction (Ex2). HPTLC on silica gel with chloroform – methanol – water 65:25:4. Detection under white light, UV 254 nm and 366 nm. Absorption densitometry measured at 190 nm. Derivatization for peptides, amino acids and amino derivatives, by immersion into ninhydrin – collidine reagent (ninhydrin 0.3 %, collidine 5 %, acetic acid 5 %, in ethanol), followed by heating 5 min at 110 °C. Effect-directed analysis using automated immersion: A) for free radical (DPPH•) scavengers; B) for enzymatic inhibition (acetyl-cholinesterase, α-glucosidase); C) for activity against Gram-negative (Aliivibrio fischeri bioluminescence assay) or Gram-positive bacteria (Bacillus subtilis bioassay). Active bands were eluted 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 200−2000) in positive and in negative ionization modes were recorded using heated electrospray ionization (HESI, spray voltage 3.5 kV, capillary temperature 270 °C). Active zones were assigned to be CLPs: iturin A, surfactin dimethyl-ester, and surfactin, fengycin and kurstakin homologues. Ex1 provided richer extracts compared to Ex2. Standards were seen to contain a free radical scavenging impurity.

      Classification: 4e, 8b, 18b, 23e
      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; gertrud.morlock@uni-giessen.de)

      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
      129 068
      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
      129 069
      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
      129 067
      Guided isolation of new iridoid glucosides from Anarrhinum pubescens by high-performance thin-layer chromatography – acetylcholinesterase assay
      E. MAHRAN, Gertrud E. MORLOCK*, M. KEUSGEN (*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, 1609, 460438 (2020). HPTLC of defatted hydro-methanolic extract of Anarrhinum pubescens (= A. duriminium) aerial parts (Plantaginaceae) on silica gel with chloroform – methanol 9:2. When intended for MS experiments, layers were previously washed twice with methanol – water 4:1 and heated 20 min at 110 °C. Derivatization by automatic piezoelectric spraying of anisaldehyde sulfuric acid reagent, followed by heating 4 min at 105 °C. Effect-directed analysis for acetyl-cholinesterase (AChE) inhibitors was performed by successive piezoelectric sprayings with TRIS buffer, with AChE solution and (after 30 min incubation at 37 °C) with naphthyl acetate and Fast Blue salt B solution. White inhibiting zones on purple background were documented under white light, and densitometry was measured by scanning in fluorescence mode at 500 nm. One of the active bands was eluted from untreated layer with methanol through the oval elution head of a TLC-MS interface pump, into a quadrupole-Orbitrap mass spectrometer using heated electrospray ionization (HESI); a full scan mass spectrum (m/z 50−750) in the positive ionization mode was recorded, as well as HRMS/MS data across a range of collision energies (10–50 V). The compound was identified as foliamenthoyl-cinnamoyl-antirrhinoside. It was applied with two other active antirrhinosides (iridoids), all isolated from the extract through column chromatography, on an HPTLC layer without migration and submitted to AChE assay; their activity was expressed as equivalency towards rivastigmine tartrate as positive control. 

      Classification: 4e, 7, 8b, 14, 32e
      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
      129 059
      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