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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      128 093
      High-throughput enzyme inhibition screening of 44 Iranian medicinal plants via piezoelectric spraying of planar cholinesterase assays
      E. AZADNIYA, I. THOMÄ, J. BAAKE, Gertrud E. MORLOCK* (*Institute of Nutritional Science, and TransMIT Center for Effect-Directed Analysis, Justus Liebig University Giessen, Giessen, Germany; gertrud.morlock@uni-giessen.de)

      Journal of Chromatography B, 1184, 122956 (2021). Test for acetyl- and butyrylcholinesterase (AChE and BChE) inhibition without development of piperin (standard inhibitor of AChE and BChE) and ethanol – water (3:2) extracts of Iranian plants, on HPTLC silica gel prewashed twice with methanol – water 3:2 and dried 60 min at 120°C. After sample application the plate was immersed (speed 3.5 cm/s, time 2 s) into enzyme solution (6.6 units/mL AChE or 3.3 units/mL BChE in TRIS buffer 0.05 M, with bovine serum albumin 0.1 %, pH 7.8), incubation 25 min at 37°C and immersion (speed 3.5 cm/s, time 1 s) into chromogenic substrate solution (α-naphthyl acetate 0.1 % and Fast Blue salt B 0.2 % in ethanol – water, 1:2). Seven mobile phases were tested for the active samples. Best separation was obtained with toluene – ethyl acetate – formic acid – water 4:16:3:2 and with toluene – ethyl acetate – methanol 6:3:1. Before enzymatic assay, plates developed with acidic mobile phases were neutralized by spraying 3 mL citrate phosphate buffer (Na2HPO4 8 %, citric acid q.s. ad pH 7.5) followed by 10 min of automatic drying. Enzymatic assay was performed using a piezoelectric spraying device: a) pre-wetting by spraying 1 mL TRIS buffer (0.05 M, pH 7.8); b) spraying 3 mL of the enzyme solution; c) incubation 25 min in a humid box at 37°C; d) spraying 0.5 mL substrate solution; e) 5 min drying at room temperature, and then 10 min of automatic drying. By spraying, zone shift and zone diffusion, which occurred with plate immersion, were avoided. For development control, derivatization was done by piezoelectrically spraying 4 mL of sulfuric anisaldehyde reagent (anisaldehyde – sulfuric acid – acetic acid – methanol, 1:10:20:170), followed by heating 3 min at 110°C. For identification of zones of interest, direct elution with methanol from underivatized HPTLC plates through a TLC-MS interface directly to a MS. Identified zones were 3-O-acetyl-β-boswellic acid (triterpenoid) from Boswellia carteri gum-resin (Burseraceae), pimpinellin and psoralen (furocoumarins) from Heracleum persicum flowers (Apiaceae), oleuropein (seco-iridoid) from Olea europaea leaves (Oleaceae), harmine, harmaline, vasicine, deoxyvasine (alkaloids) from Peganum harmala seeds (Zygophyllaceae), costic acid (sesquiterpene) from Nardostachys jatamansi hypocotyl (Valerianaceae), elaidic, linoleic, palmitic, palmitoleic acids (fatty acids) from Pistacia atlantica fruits (Anacardiaceae).

      Classification: 4e, 8b, 11a, 15a, 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
      128 048
      Cholestasis impairs hepatic lipid storage via AMPK and CREB signaling in hepatitis B virus surface protein transgenic mice
      K. IRUNGBAM, M. RODERFELD, H. GLIMM, F. HEMPEL, F. SCHNEIDER, L. HEHR, D. GLEBE, Y. CHURIN, G. MORLOCK, I. YÜCE, Elke ROEB* (*Department of Gastroenterology, Justus Liebig University Giessen, Giessen, Germany; elke.roeb@innere.med.uni-giessen.de)

      Nature - Lab. Invest. 100, 1411–1424 (2020). Samples were chloroform – methanol 1:1 solutions of lipid standards and of liver tissue extracts from wild-type mice (1), from transgenic murine models of hepatic steatosis (2) (mice expressing HBs, hepatitis B virus surface protein), or of cholestasis (3) (mice totally knock-out for the gene of phospholipid translocator ABCB4, ATP-binding cassette subfamily B member 4), or of both (4) (hybrids of mice (2) and (3)). HPTLC on silica gel (preheated at 110°C for 15 min) with n-hexane – diethyl ether – acetic acid 20:5:1. (A) For qualitative analysis, visualization under white light after immersion into anisaldehyde 0.5 % (in sulfuric acid – acetic acid – methanol, 1:2:17), followed by heating at 110°C for 9 min. (B) Identification of lipids was confirmed by elution of the zones of interest with methanol from the HPTLC layer through a TLC-MS interface and a filter frit directly to a quadrupole-orbitrap MS (atmospheric pressure chemical ionization, full HR-MS scan in m/z range 100–1000). (C) For quantitative analysis, visualization at UV 366 nm after derivatization by immersion into primuline reagent (primuline 0.5 g/L in acetone – water 4:1); fluorescence was measured at UV 366 nm (mercury lamp, optical filter for wavelengths above 400 nm, scanning slit 6.0 mm × 0.2 mm, speed 20 mm/s). (A) and (B) allowed the separation and detection of cholesterol, cholesteryl oleate, methyl oleate, free fatty acids (FFA, expressed as oleic acid equivalents) and triacylglycerols (TAG, as triolein equivalents) in liver extracts. (C) showed that TAG was decreased and FFA increased in (3) and (4), compared to (1) and (2). Cholesterol and cholesteryl oleate had no significant changes between groups.

      Classification: 4e, 11a, 11c, 13c
      128 005
      Quaternion-based parallel feature extraction: Extending the horizon of quantitative analysis using TLC-SERS sensing
      Y. ZHAO (Zhao Yong), A. TAN (Tan Ailing), K. SQUIRE, K. SIVASHANMUGAN, A. WANG (Wang Alan)* (*School of Electrical Engineering and Computer Science, Oregon State University, Corvallis, OR, 97331, USA, wang@eecs.oregonstate.edu)

      Sens. Actuators. B. Chem. 299, 126902 (2019). TLC-surface-enhanced Raman scattering (TLC-SERS) of melamine contaminated milk samples on silica gel with acetone - chloroform - ammonia 14:1:4. Then 2 μL gold nanoparticle were drop onto the analyte spot. Quantification using a Raman microscope equipped with a CCD detector to acquire the surface-enhanced Raman scattering spectra. Excitation wavelength was 785 nm. A parallel representation model of the triple-spectral data was constructed using a pure quaternion matrix. Quaternion principal component analysis (QPCA) was utilized for feature extraction and followed by feature crossing between the quaternion principal components to obtain final fusion of spectral feature vectors.

      Classification: 4e
      128 014
      Applications of direct analysis in real time mass spectrometry in food analysis: A review
      X. ZHANG (Zhang Xiaoping), A. REN (Ren Xiang), K. CHINGIN* (*Jiangxi Key Laboratory for Mass Spectrometry and Instrumentation, East China University of Technology, Room 804, Science & Technology Building, 418 Guanglan Road, Nanchang City, Jiangxi Province 330013, China, chingin.k@gmail.com)

      Rapid Commun. Mass Spectrom. 35, 9013 (2021). Review of the application of direct analysis in real time (DART) combined with mass spectrometry (MS) detection in food science and industry published in the period from 2005 to this date. The applications described the use of HPTLC in preparation methods as well as the combination of HPTLC fingerprints and DART-MS with multivariate data analysis for the differentiation of natural propolis products.

      Keywords: HPTLC review
      Classification: 1b, 4e
      128 049
      High-throughput planar solid-phase extraction coupled to orbitrap high-resolution mass spectrometry via the autoTLC-MS interface for screening of 66 multi-class antibiotic residues in food of animal origin
      A. MEHL, L. SCHMIDT, L. SCHMIDT, Gertrud MORLOCK* (Chair of Food Science, Institute of Nutritional Science, and Interdisciplinary Research Center, Justus Liebig University Giessen, Heinrich-Buff-Ring 26-32, 35392 Giessen, Germany, gertrud.morlock@uni-giessen.de)

      Food Chem. 351, 129211 (2021). High-throughput planar solid-phase extraction of 66 multi-class antibiotic residues in muscle tissue, cow milk and chicken eggs on silica gel with acetonitrile - methanol - ammonia 5:3:2 as first front-elution up to 85 mm followed by a second front-elution in the reverse direction up to 25 mm with acetonitrile -water - ammonia 9:7:4. Evaluation under UV 254 nm and 366 nm. Detection of macrolides by spraying with p-anisaldehyde sulfuric acid reagent (methanol - glacial acetic acid - sulfuric acid - p–anisaldehyde 420:50:26:3), followed by heating at 110°C for 3 min. Detection of penicillins by spraying with ninhydrin reagent (500 mg ninhydrin in ethanol - glacial acetic acid 23:2). Detection of lincosamines by spraying with aniline diphenylamine o-phosphoric acid reagent (2 g diphenylamine in methanol – o-phosphoric acid - aniline 90:10:1). Via simple clicks on the image, the auto TLC-MS interface automatically eluted the target zones at the trace level from the TLC plate into a Q Exactive Plus Hybrid Quadrupole-Orbitrap Mass Spectrometer.

      Classification: 4e, 28a
      127 027
      Fast screening and quantitative mass spectral imaging of thin-layer chromatography plates with flowing atmospheric-pressure afterglow high-resolution mass spectrometry
      C. KUHLMANN, M. HEIDE, C. ENGELHARD* (*Department of Chemistry and Biology, University of Siegen, Adolf-Reichwein-Str. 2, 57076 Siegen, Germany, engelhard@chemie.uni-siegen.de)

      Anal. Bioanal. Chem. 411, 6213-6225 (2019). HPTLC of selected analgesics (acetaminophen), alkaloids (nicotine and caffeine), and steroids (cortisone) on different
      stationary phases (silica gel, RP-, cyano-, DIOL- and amino-) with isopropyl alcohol - n-heptane - water 7:3:1. Direct surface analysis of the TLC plates with a flowing atmospheric pressure afterglow (FAPA) ambient desorption/ionization source (TLC-FAPA-MS). The LOD of caffeine was 0.6 ng/zone. Semi-polar stationary phases (cyano and RP plates) showed significantly higher signal abundances for the analyzed compounds in comparison to the polar NP stationary phase.

      Classification: 4e
      127 005
      Utilization of a crown ether/amine‐type rotaxane as a probe for the versatile detection of anions and acids by Thin‐Layer Chromatography.
      S. MIYAGAWA, M. KIMURA, S. KAGAMI, T. KAWASAKI, Y. TOKUNAGA* (*Department of Materials Science and Engineering, University of Fukui, Bunkyo, Fukui, Japan; tokunaga@u-fukui.ac.jp)

      Chem. Asian J. 15(19), 3044-3049 (2020). The studied rotaxane combines a dibenzocrown of 8 ethers (DB24C8) with an axle chain (Ax) containing two amines, one of them in an aniline group, allowing stability of the rotaxane even when the other one is unprotonated. TLC on silica gel in 4 steps, with detection under UV light or after derivatization with phosphomolybdic acid in ethanol. (1) Before the synthesis of the rotaxane, unprotonated Ax was isolated by preparative TLC of the protonated Ax obtained by addition of HCl or toluenesulfonic acid (TsOH); the mobile phases were chloroform – methanol 10:1 and toluene – tetrahydrofurane 3:2, respectively. The isolated molecules were confirmed as totally unprotonated Ax by NMR, suggesting a complete loss of HCl and TsOH on the silica gel layer. (2) After synthesis, unprotonated rotaxane, pure vs. monoprotonated by the addition of 10 different acids (and purified by column chromatography CC), was applied on TLC plates and developed with dichloromethane – acetone – water 3:16:1; the hRF values were very different, depending on the counter-anions from the used acids. (3) The same behavior (except with sulfuric acid) was observed under the same conditions when CC was omitted (unprotonated rotaxane samples were mixed with each of the acids, or with two acids at the same time for acid-competitive TLC analysis). (4) When unprotonated rotaxane was applied under the same conditions as in step (3) with the sodium salts instead of the acids, the behavior was similar (except for the shapes of the spots, due to the salts in excess). The rotaxane can thus be used for the TLC separation and detection of sodium salts, by forming salts of protonated rotaxane with the anion afforded by these sodium salts. The rotaxane protonation seems to be promoted by the methanol of the spotting mixture; indeed, when step (3) was performed with the mobile phase chloroform – methanol 10:1, a second zone appeared because methanol formed a salt with the rotaxane (identified by NMR).

      Classification: 4e, 5a, 5b, 17a