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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      130 094
      Baobab pulp authenticity and quality control by multi-imaging high-performance thin-layer chromatography
      J. CHEPNGENO, S. IMATHIU, W. OWINO, Gertrud MORLOCK* (*Institute of Nutritional Science, Chair of Food Science, and Interdisciplinary Research Center (iFZ), Justus Liebig University Giessen, Heinrich-Buff-Ring 26-32, 35392 Giessen, Germany, gertrud.morlock@uni-giessen.de)

      Food Chem. 133108 (2022). HPTLC of 135 baobab samples (Adansonia digitata) from different agroecological regions on silica gel with toluene - ethyl acetate - methanol - formic acid - water 60:50:25:3:5. Detection by dipping into aniline diphenylamine o-phosphoric acid reagent, p-amino benzoic acid reagent, or p-anisaldehyde sulfuric acid reagent, followed by heating at 120 °C for 5 min. Qualitative analysis under UV light at 254 nm. fluorescence detection at 366 nm and white light illumination. 

       

      Classification: 32e
      130 031
      An efficient and quick analytical method for the quantification of an algal alkaloid caulerpin showed in-vitro anticancer activity against colorectal cancer
      N. MERT-OZUPEK, G. CALIBASI-KOCAL, N. OLGUN, Y. BASBINAR, L. CAVAS, Hulya ELLIDOKUZ* (*Department of Preventive Oncology, Institute of Oncology, Dokuz Eylül University, Izmir, Turkey; hulya.ellidokuz@deu.edu.tr)

      Marine Drugs 20(12), 757 (2022). Samples were ethyl acetate macerates and diethyl ether Soxhlet extracts from invasive Caulerpa cylindracea and non-invasive C. lentillifera (Caulerpaceae), as well as caulerpine (bisindole alkaloid) as standard isolated from one of the extracts. TLC on silica gel with petroleum ether – diethyl ether 1:1. Quantitative evaluation by densitometry at 330 nm, quantification of caulerpine (hRF 41, LOD 20 ng/zone, LOQ 68 ng/zone). The concentrations of caulerpine in C. cylindracea extracts (96-112 µg/g) were higher than in C. lentillifera (0-8 µg/g).

      Classification: 22, 32e
      130 030
      High-performance thin-layer chromatography hyphenated with microchemical and biochemical derivatizations in bioactivity profiling of marine species
      Snezana AGATONOVIC-KUSTRIN*, E. KUSTRIN, V. GEGECHKORI, D. W. MORTON (*Department of Pharmaceutical and Toxicological Chemistry, Institute of Pharmacy, Sechenov University, Moscow, Russia, and School of Pharmacy and Biomedical Sciences, La Trobe Institute for Molecular Sciences, La Trobe University, Bendigo, Australia; s.kustrin@latrobe.edu.au)

      Marine Drugs 17(3), 148 (2019). Samples were ethyl acetate extracts of seagrass Amphibolis antarctica (Cymodoceaceae), and of algae: Austrophyllis harveyana (Kallymeniaceae), Carpoglossum confluens, Cystophora harveyi, C. monilifera, C. pectinata and C. subfarcinata, Myriodesma integrifolium, Sargassum lacerifolium (Sargassaceae), Codium fragile subsp. tasmanicum (Codiaceae), Ecklonia radiata (Lessoniaceae), Hypnea valida, Rhodophyllis membaneacea (Cystocloniaceae), Hormosira banksii (Hormosiraceae), Perithalia caudata (Sporochnaceae), Phyllospora comoasa, Scytothalia dorycarpa (Seirococcaceae), Plocamium dilatatum (Plocamiaceae), and epiphytic brown algae. HPTLC on silica gel (pre-washed with methanol and heated 30 min at 100 °C) with n-hexane – ethyl acetate – acetic acid 15:9:1. Derivatization by immersion: A) into anisaldehyde – sulfuric acid reagent, followed by 10 min heating at 105 °C, for the detection of steroids and terpenes; B) into DPPH• (0.2 % in methanol), followed by 30 min incubation in the dark, for the detection of antioxydants; C) into Fast Blue B solution (0.1 % in 70 % ethanol) for detection of phenols (with alkylresorcinols detected as dark purple zones on colorless background). Effect-directed analyses were performed directly on the plates. D) α-Amylase inhibition assay by immersion into enzyme solution, incubation 30 min at 37 °C, immersion into substrate solution (starch 2 % in water), incubation 20 min at 37 °C and immersion into Gram’s iodine solution for detection (inhibition zones appear blue on white background). E) Acetylcholinesterase (AChE) inhibition assay (after neutralization by immersion into phosphate buffer) by immersion into enzyme solution, incubation 30 min at 37 °C, immersion into substrate solution (α-naphthyl acetate) and into dye reagent (Fast Blue Salt B). Densitometry through automated scanning, quantification expressed as equivalents to the respective standards used for calibration curves: A) β-sitosterol (LOQ 1.6 µg/band), B) gallic acid (LOQ 60 ng/band), D) acarbose (LOQ 173 µg/band), E) donepezil (LOQ 96 µg/mL). Alkylresorcinols were detected as antioxydant in C. harveyi and C. pectinata (hRF 88), and in C. subfarcinata (hRF 72, 81, 88). Enzymatic inhibitors in C. fragile were considered as a flavone (hRF 65) and a terpenoid (hRF 77), due to their absorption curves (densitometric scan in range 200-400 nm).

      Classification: 4e, 7, 8a, 15a, 32e
      130 029
      Efficient isolation of mycosporine-like amino acids from marine red algae by fast centrifugal partition chromatography
      M. ZWERGER, S. SCHWAIGER, M. GANZERA* (*Department of Pharmacognosy, Institute of Pharmacy, University of Innsbruck, Innsbruck, Austria; markus.ganzera@uibk.ac.at)

      Marine Drugs 20(2), 106 (2022). TLC was used to monitor the fractionation of hydro-methanolic extracts of Rhodophytes: Gracilaria gracilis (Gracilariaceae) (A), Porphyra sp. (Bangiaceae) (B), Spongoclonium pastorale (Ceramiaceae / Wrangeliaceae) (C); and to assess the purity of two isolated mycosporine-like amino acids: porphyra-334 and shinorine.  TLC on silica gel with n-butanol - acetic acid - water 3:1:1. Derivatization by spraying ninhydrin reagent for the detection of peptides and amino-acids; or by spraying anisaldehyde - sulfuric acid for most phytochemicals; in both cases, followed by 5 min heating at 100 °C. Visualization under white light and at 366 nm. Porphyra-334 (hRF 28) was isolated pure from (B) and (C). Shinorine (hRF 25), isolated from (A) and (B), contained a coeluting sugar (hRF 48), which was absent after further purification on solid phase extraction, and, only when isolated from (B), a coeluting peptide or amino-acid (hRF 35), which was absent after further purification on cyclodextrane column chromatography.

      Classification: 4d, 18a, 32e
      130 106
      Characterization of quality differences of Ophiopogonis Radix from different origins by TLC, HPLC, UHPLC-MS and multivariate statistical analyses
      L. JIANG (Jian Ling), Y. QIU (Qiu Yixing), Z. CHEN (Chen Zhuliang), L. LUO (Luo Lu), H. TANG (Tang Hongxia), X. ZHOU (Zhou Xudong), H.YUAN (Yuan Hangwen), W. WANG (Wang Wei)*, P. LIU (Liu Pingan) (*TCM and Ethnomedicine Innovation and Development International Laboratory, School of Pharmacy, Hunan University of Chinese Medicine, Changsha, Hunan 410208, China, wangwei402@hotmail.com)

      J. Liq. Chromatogr. Relat. Technol. https://doi.org/10.1080/10826076.2022.2159977 (2021). HPTLC of Ophiopogonis Radix from different habitats on silica gel with toluene - methanol - glacial acetic acid 800:50:1. Detection under UV light at 254 nm. 

       

      Classification: 32e
      130 028
      The effect of extractive lacto-fermentation on the bioactivity and natural products content of Pittosporum angustifolium (gumbi gumbi) extracts
      Snezana AGATONOVIC-KUSTRIN*, V. GEGECHKORI, D.W. MORTON
      (*Department of Pharmaceutical and Toxicological Chemistry, Institute of Pharmacy, Sechenov University, Moscow, Russia, and School of Pharmacy and Biomedical Sciences, La Trobe Institute for Molecular Sciences, La Trobe University, Bendigo, Australia; s.kustrin@latrobe.edu.au)

      J Chromatogr A, 1647, 462153 (2021). Samples were extracts of Pittosporum angustifolium leaves (Pittosporaceae), either pure or fermented 1-4 weeks in NaCl solution, as well as acarbose, gallic acid, β-sitosterol, caffeic and chlorogenic acids, as standards. HPTLC on silica gel (prewashed with methanol and dried 15 min at 105 °C) with n-hexane – ethyl acetate – acetic acid 15:9:1. Derivatization by immersion (speed 5 cm/s, time 1 s): (A) into DPPH• 0.2 % solution, to detect radical scavengers; (B) into neutralized ferric chloride (3 % in ethanol), followed by 5 min heating at 110 °C, for detection of phenolic compounds; (C) into anisaldehyde – sulphuric acid reagent, followed by 10 min heating at 110 °C, to detect terpenes and steroids. Effect-directed analysis (EDA) for α-amylase inhibition assay (D) by immersion into enzyme solution, incubation 15 min at 37 °C, immersion into substrate solution (starch 2 % in water), incubation 20 min at 37 °C and immersion into Gram’s iodine solution for detection (inhibition zones appear blue on white background). In all cases, visualization under white light. Quantification was performed on pictures using image processing software, and expressed as equivalents to the respective standards used for calibration curves: (A) and (B) gallic acid (LOQ 250 and 740 ng/band, respectively), (C) β-sitosterol (LOQ 1.5 µg/band), (D) acarbose (LOQ 8 µg/band). Zones of interest, scraped from untreated plates and washed with ethyl acetate, were submitted by ATR-FTIR analysis. An amylase inhibiting zone (hRF 85) present in all extracts was identified as fatty acid esters: ethyl palmitate in unfermented and methyl linoleate in fermented extracts. Moreover, fermented extracts contained antioxidant zones (hRF 15 – 20), identified as monomers and oligomers (including hydroxycinnamic, guaiacyl, syringyl derivatives) from decomposed lignin.

      Classification: 4e, 7, 8b, 11a, 32e
      130 013
      Characterization of natural herbal medicines by thin-layer chromatography combined with laser ablation-assisted direct analysis in real-time mass spectrometry
      Y. CHEN (Chen Yilin), L. LI (Li Linnan)*, R. XU (Xu Rui), F. LI (Li Fan), L. GU (Gu Lihua), H. LIU (Liu Huwei), Z. WANG (Wang Zhengtao), L. YANG (Yang Li)** (*Shanghai Key Laboratory of Compound Chinese Medicines, and Institute of Chinese Materia Medica, Shanghai University of Traditional Chinese Medicine, Shanghai, China; **Institute of Interdisciplinary Integrative Medicine Research, Shanghai University of Traditional Chinese Medicine, Shanghai, China; *linnanli@shutcm.edu.cn, **yl7@shutcm.edu.cn)

      J Chromatogr A, 1625, 461230 (2020). Samples were extracts of Chinese plants: Acorus tatarinowii (= Acorus calamus var. angustatus) rhizomes (Araceae / Acoraceae) (1), Angelica sinensis roots (Apiaceae) (2), Gynura japonica rhizomes (Asteraceae) (3), Phellodendron chinense bark (Rutaceae) (4), Picrasma quassioides twigs and leaves (Simaroubaceae) (5), Rheum sp. roots and rhizomes (R. palmatum, R. tanguticum and/or R. officinale) (Polygonaceae) (6), Sophora flavescens roots (Fabaceae) (7), Dendrobium stems (D. aphyllum, D. aurantiacum var. dennaeanum, D. chrysanthum, D. chrysotoxum, D. gratiosissimum, D. hercoglossum, D. thyrsiflorum, D. trigonopus and D. williamsonii) (Orchidaceae) (8). Standards were: gigantol (from D. sonia); methoxycarbonyl-β-carboline (MCC from (5)); caffeic acid, emodin; senecionine and β-asarone; crategolic acid (= maslinic acid), corosolic acid, oleanic acid, ursolic acid; sesquiterpenoids (atractylenolides I – III) from Atractylodes macrocephala (Asteraceae); flavonoids (baicalein, baicalin, daidzin, hesperidin, wogonin) from Scutellaria baicalensis roots (Lamiaceae). HPTLC on silica gel with 10 mobile phases, depending on the samples. Detection under UV 254 nm and white light. For (3), derivatization with Dragendorff’s reagent (bismuth potassium iodide solution) for visualization of alkaloids. Zones of interest on underivatized plates were identified by a triple-quadrupole ­– linear ion-trap MS, the compounds being removed from the layer by a continuous-wave (445 nm) diode laser pointer through a DART interface (Direct Analysis in Real-Time, helium as gas for plasma-based ambient ionization, discharge needle voltage 1.5 kV, grid voltage 350 V, capillary temperature 300 °C and voltage 40 V, full scan in positive ionization mode in m/z range 150-800). Pigment standards were used for validation of this laser-assisted HPTLC-DART-MS method: malachite green, crystal violet, chrysoidin, auramine O, rhodamine B, Sudan red I – IV, Sudan red G, dimethyl yellow. Afterwards, the same HPTLC-MS method was applied to the origin / species determination of Dendrobium samples, based on the presence of four bibenzyl compounds erianin, gigantol, moscatilin, tristin. Erianin was present only in D. chrysotoxum, whereas none of these were detected in D. hercoglossum. Several components of the extracts were thus identified: asarone (a phenylpropanoid) in (1); phthalide lactones (butenylphthalide, ligustilide and chuanxiong lactone) in (2); co-eluting pyrrolizidine alkaloids (senecionine and seneciphylline) in (3); benzylisoquinoline alkaloid berberine in (4); alkaloids (canthinone alkaloids and MCC) in (5); anthraquinones (rhein, aloe-emodin, emodin, emodin methyl ether, chrysophanol) and (in negative mode) caffeic acid (a hydroxycinnamic acid) and corosolic, maslinic and oleanic acids (triterpenoids) in (6); quinolizidine alkaloids (matrine, oxymatrine, oxysophocarpine, sophoridine) in (7).

      Classification: 4e, 7, 8a, 8b, 15a, 22, 32e
      130 027
      Thin-layer chromatographic quantification of magnolol and honokiol in dietary supplements and selected biological properties of these preparations
      E. LATA, A. FULCZYK, P.G; OTT, T. KOWALSKA, M. SAJEWICZ, Ágnes M. MÓRICZ* (*Plant Protection Institute, Centre for Agricultural Research, 1022 Budapest, Hungary; moricz.agnes@agrar.mta.hu)

      J Chromatogr A, 1625, 461230 (2020). Samples were methanolic extracts of commercial supplements containing Magnolia sp. bark (Magnoliaceae), as well as honokiol (1) and magnolol (2) (biphenyl neolignans) as separated or mixed standards. TLC and HPTLC on silica gel with n-hexane – ethyl acetate – ethanol 16:3:1. Visualization under UV 254 nm. Quantification of (1) and (2) by densitometric scanning in absorbance mode at 290 nm (hRF were 34 and 39, LOQ 200 ng and 280 ng/spot, respectively). Variability between samples from the same brand supplement was also determined, as well as extraction yields. Effect-directed analysis with 3 assays: A) to detect radical scavengers, immersion into DPPH• 0.02 % solution; B) to detect activity against Gram-negative bacteria, immersion into Aliivibrio fischeri suspension, followed by recording the bioluminescence; C) to detect activity against Gram-positive bacteria, immersion into Bacillus subtilis, followed by incubation 2 h at 28 °C and immersion into MTT 1 g/L. Compounds (1) and (2) were active in all assays. Identification of zones of interest by eluting with methanol from untreated TLC layer through the oval elution head of a TLC-MS interface directly to a single Quadrupole MS (electrospray ionization, interface temperature 350°C, heat block temperature 400°C, desolvation line temperature 250°C, detector voltage 4.5kV). Full mass scan spectra were recorded in the positive and negative ionization modes in m/z range 150–800. Other molecules (from other ingredients) were identified: piperine (alkaloid) and/or its geometrical isomers (active on A, hRF 29-30); and daidzein (active on A and B, hRF 18), isoflavone from Pueraria montana root (Fabaceae). Stability was assessed through 2D-HPTLC, by repeating the same development method in the orthogonal direction 4 h or 20 h after the first separation. Degradation products of (1) and (2) appeared after 20 h (but not at 4 h), including a honokiol dimer (formed in tracks of (1) and of (2)).

      Classification: 4e, 7, 8a, 22, 32e
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